Abstract:
The present invention discloses a portable, reliable, automated and simple device using Spectral Fluorescence Signature technology (SFS) for fast and accurate drug detection, quantification and data storage. The present also discloses a method for using Spectral Fluorescence Signature technology (SFS) for fast and accurate drug detection, quantification and data storage. Such device and method needing not highly skilled personnel or specific background to run the tests.

Description:
FIELD OF THE INVENTION 
     This invention relates the use of Spectral Fluorescence Signature technology (SFS) for on-site drug detection and quantification. 
     BACKGROUND OF THE INVENTION 
     Testing and quantifying street samples, for example for narcotics, with the current devices and methods known in the art, although some times very precise, still takes a long time and requires personnel with specific scientific backgrounds. Accordingly, legal actions and court proceedings depending on those analysis are frequently dismissed. Detection and quantification of street samples, including powder or solid form, or as crushed dried plants, or as tobacco from cigarettes (cigars), or in a liquid form is a complex task due to multi component samples constituting drug mixtures with adulterants and diluents in different ratios. Many devices known in the prior art for drug detection and quantification are bench top laboratory equipments. These are sophisticated equipments that, although precise, are costly and require a sample preparation step, a long time for issue of a result and require highly trained personnel to run the tests. 
     Some devices for drug detection, which are portable devices, are intended for detecting trace drug samples, which is not the purpose of this invention. These devices are limited to detecting specific (single) drug traces, mainly because these equipments cannot identify mixtures of unknown composition. 
     Three technologies are used at present for the task of street drug detection: Raman spectroscopy, infra red spectroscopy and fluorescence. 
     Although Raman spectroscopy is suitable for field operation, the selectivity in mixtures is doubtful and the data interpretation is questionable. Three major shortcomings limit the use of Raman spectroscopy for qualitative and quantitative analysis. Fluorescence is the major problem as even low levels of fluorescence can mask the Raman signal. The second problem arises due to absorbance effects of different components in such samples. The third problem is that because complex samples are studied in bulk, it is challenging to determine the identity of each compound when multiple peaks from several compounds are present in the same spectral region. Therefore the use of Raman spectroscopy in the investigation of colored samples or highly fluorescing and multi component sample is difficult. False results are frequent consequences of this situation. 
     The use of infrared spectroscopy is doubtful because the known device based on this technology is proposed for identification of drugs and other chemicals in clandestine labs, meaning that samples are not the real complex street samples with adulterants and diluents. Several shortcomings are known in this technology, such as that low energy flow of light sources in the infrared spectral range causes low sensitivity and low selectivity of this technique. Also, the numerous absorptions bands of solvent and water vapor in the air influence the interpretation of results. Furthermore, adulterants and diluents make the analysis of street drugs practically impossible without a complex preparation of the samples. 
     Fluorescence is a well known technology for the detection of organic substances and mixtures in various matrixes. However, presently there is no device or method aimed for the analysis of street drugs based on this technology, due to the specific spectral characteristics of street drugs as seen below:
         complex and multi component character of the samples hampers analysis by conventional fluorescence techniques without preliminary separation of the components;   spectra overlapping and non-additive combination of fluorescence intensities caused by possible mutual interaction of the components;   variability of the fluorescent characteristics of the mixed sample caused by possible adulterants and diluents, and   necessity to detect, or detect and quantify, simultaneously several components in a mixed sample.       

     Patents of the prior art for drug detection use different methodologies. For example, U.S. Pat. No. 5,648,047 to Kardish et al. and U.S. Pat. No. 4,840,912 to Glattstein disclose the use of color tests. U.S. Pat. No. 4,812,413 to Glattstein et al., U.S. Pat. No. 4,196,167 to Olsen and U.S. Pat. No. 6,194,898 to Magnuson et al., all use different kinds of methods, devices or kits. 
     In view of the foregoing, for a better and faster response to investigations and law enforcement actions, it is desirable that street samples to be diagnosed for the presence of narcotics and other components (if necessary) on-site by police officers, customs officers and others, using a simple and quick procedure without any requirement for special education or long training. There is also a demand for a method of, and a portable device for, detection of drugs in street samples where manual operations have to be minimized, simplified and able to be repeated. Further more, the proper preparation of the samples for correct measurements has to be done automatically, the detection accuracy has to be in accordance with the acting cut off levels as false positive and false negative results may result in inappropriately charging a person or with the possibility of missing a crime. Finally, analysis data have to be documented, safely stored and possibly transferred to a different site. 
     SUMMARY OF THE INVENTION 
     The present invention seeks to provide a device and a method of outstanding optical differentiation, recognition, detection and quantification together with a data storage capacity concerning one or several substances in a complex mixtures without preliminary separation and chemicals. 
     The present invention seeks to provide a portable, reliable, automated and simple device using Spectral Fluorescence Signature technology (SFS) for fast and accurate drug detection, quantification and data storage. The present invention also seeks to provide a method using Spectral Fluorescence Signature technology (SFS) for fast and accurate drug detection, quantification and data storage. Such device and method needing not highly skilled personnel or personnel with a specific scientific background to run the tests. Ideally, the method and device of this invention require no more skill and training than to required by a police officer using a breathalyzer. In one aspect of the invention, the present invention seeks to provide a portable device for detection and quantification of drugs in street samples including:
         -CLAIM  1  will be inserted here before filing-       

     For purposes of discussion, street samples in this application are the forms of illegal traffic and sell of drugs of abuse. They are usually presented by mixture of drugs of abuse with adulterants and diluents at different ratio. Sometimes they may contain only adulterants and diluents without drugs of abuse. Among adulterants of street samples may be toxic substances in high concentrations. 
    
    
     
       BRIEF DESCRIPTION OF THE DRAWINGS 
         FIG. 1  is a block diagram of the device of the present invention; 
         FIG. 2  is a plan schematic view of a first embodiment of the optical layout having a cell for liquid samples; 
         FIG. 3  is a partial sectional view generally taken along the line A-A of  FIG. 2 ; 
         FIG. 4  is partial sectional view generally taken along the line B-B of  FIG. 2 ; 
         FIG. 5  is a plan schematic view of a second embodiment of the optical layout having a container for dense samples; 
         FIG. 6  is a partial sectional view generally taken along the line C-C of  FIG. 5 ; 
         FIG. 7  is a partial sectional view generally taken along the line D-D of  FIG. 6 ; 
         FIG. 8  is a partial sectional view generally taken along the line E-E of  FIG. 6 . 
         FIG. 9   a  is a diagrammatic representation of a Spectral Fluorescent Signature. 
         FIG. 9   b  is a diagrammatic representation of the absorption matrix. 
         FIG. 10  is a diagrammatic representations of the recognition and quantification method. 
     
    
    
     DETAILED DESCRIPTION OF THE INVENTION 
     The technology of Spectral Fluorescence Signatures (SFS) is effectively applied for detection and identification of organic impurities in a water matrix. This technique offers a 3-dimensional fluorescent pattern display of the sample. The three dimensions are: excitation wavelengths, emission wavelengths, and fluorescent intensity. These patterns can also be presented in a 2-dimensional spectral image of equal fluorescence intensity levels.  FIG. 9   a  is showing a diagrammatic representation of a Spectral Fluorescent Signature presented in a 2-dimensional spectral image where EM is emission wavelengths and EX is excitation wavelengths, showing the different fluorescent intensity levels.  FIG. 9   b  is a diagrammatic representation of the absorption matrix, which represents the values of optical absorption in the sample for every element of the SFS matrix. Different substances are revealed in different positions in the matrixes. 
     It is important to note that the level of fluorescent intensity is directly proportional to the amount, or concentration, of the compounds present in the mixture. 
     Since every chemical substance that has feature to emit the fluorescence has its own characteristic excitation and emission wavelengths, different substances generate different SFSs. The SFSs of the sought substances are previously measured and stored in the library for later reference. The fluorescent patterns of the untreated street sample being measured can then be compared to the SFS of these known library substances. 
     In this way, different substances in a mixture can be recognised and quantified without requiring any reagents for sample preparation (or with a minimal preparation procedure). Another advantage of this library is that the background fluorescence as SFS is also measured. If the background fluorescence is fluctuating, it is taken into account by the expert system, thereby providing a more consistent and reliable result, as can be seen in  FIG. 10  where a diagrammatic representations of the recognition and quantification method is shown. 
     The optical density of liquid samples that is controlled by photometric measurements is important feature of sample and is taken in account for calibration of fluorescence intensity versus concentration of the substances. 
     The following modifications on the SFS technique allow its use for the detection of drugs in street samples:
         an additional spectral channel is used to measure absorption spectra in the analyzed sample—to take into account the influence of the non-fluorescing or highly absorbing components;   the absorption value is measured simultaneously with the fluorescence intensities at every step of excitation wavelength—to take into account possible photochemical processes;   the excitation, emission and absorption spectral windows and resolution are selected and fixed in a way to cover specific excitation/emission fluorescence and absorption bands of all major drugs, adulterants and diluents—it provides reliable screening of unknown composition in a sample for drug detection;   the measured SFS is accompanied with an absorption matrix (AM), and SFS &amp; AM are treated as a united result of the measurement—AM adds one more dimension to 3-dimensional SFS in the information matrix, and therefore provides components recognition, when interaction between components takes place, and   the united result (SFS &amp; AM) are processed by computer system based on combination of preliminary prepared spectral library and specialized software consisting of identification, interaction verification and automatic calibration modules.       

     The device of this invention, as shown in  FIG. 1 , includes optically connected an ultraviolet-visible (UV-VIS) light source  1 , a condenser/filter assembly  2  with filter drive  3 , an excitation monochromator  4  with diffraction grating drive  5  (e.g. stepper motor), a reference photo-detector  6 , a wavelength calibration photo-detector  7 , a cell assembly  8 , an absorption photo-detector  9  for absorption spectra measurements, an emission monochromator  10  with diffraction grating drive  11 , a wavelength calibration light source  12 , and an emission photo-detector  13 . A microcontroller unit (controlling means)  14  is provided for device controlling, data processing, and communication with an external computer via different link types. Communicating periodically with grating drives  5  and  11 , wavelength calibration photo-detector  7  of the excitation monochromator  4 , wavelength calibration light source  12  of the emission monochromator  10 , and emission photo-detector  13 , the microcontroller  14  performs a task of self-calibration of wavelength scales of both scanning monochromators  4  and  10  providing advanced reliability of the device in fieldwork conditions (transport shocks, vibration, etc). The diffraction grating drives  5  and  11  are preferably stepper motors. 
     The plan schematic view of the first embodiment of the optical layout having a cell for liquid samples is shown in  FIG. 2 . Optical system includes a light source  1 , e.g. a Xenon discharge lamp, a collimator lens  16  collecting light from the light source  1  and forming a collimated light beam further focused by a focusing lens  18  onto the entrance slit  19  of the excitation monochromator. As an option a longpass optical filter  17  may be inserted between the collimator lens  16  and focusing lens  18  for cutting off the higher spectral orders present when working in a wide excitation wavelength range from UV to VIS spectrum. Most of the light passed through the entrance slit  19  passes through a plate beamsplitter  20  placed into the diverging light beam at an angle of incidence of 45° and is reflected by a beam inclining plane mirror  21  to a concave diffraction grating  22 . The beam-inclining mirror  21  is intended for saving space and makes possible the more compact design of the device. 
     In the first embodiment the diffraction grating  22  is a holographically recorded aberration corrected concave grating with varied groove spacing and curved grooves, the grating being turnable for wavelength scanning around the vertical axis  23  passing through the grating vertex. The use of an aberration corrected holographic grating leads to a simple and compact mechanical design and provides good spectral image quality on the monochromator exit slit  25  plane over a wide spectral range from UV to VIS. Diffracted and converged by the diffraction grating  22 , a light beam of a particular wavelength determined by the grating rotation angle is reflected by a beam inclining mirror  24  towards the monochromator exit slit  25  placed at the locus of the best quality spectrum. 
     Outgoing through the exit slit  25  a diverging light beam is collimated by a lens  28  and passes through a cell  29  filled with liquid sample  30 . Fluorescence light emitted from the sample  30  at an angle of 90° from the excitation beam direction is bent by means of a right angle prism  31  by 90° and focused by a lens  32  onto the entrance slit  33  of the emission monochromator. The diverging light beam passed through the entrance slit  33  is reflected by a beam inclining plane mirror  34  to a concave diffraction grating  37 . 
     In the first embodiment the diffraction grating  37  is a holographically recorded aberration corrected concave grating with varied groove spacing and curved grooves, the grating being turnable for wavelength scanning around the vertical axis  38  passing through the grating vertex. Diffracted and converged by the diffraction grating  37 , a light beam of a particular wavelength determined by the grating rotation angle is focused on the plane of the exit slit  39 . A photo-detector  13  located behind the slit  39  serves to measure of emission spectra of fluorescence. The photo-detector  13  is preferably a photomultiplier tube. 
     An absorption photo-detector  9  located behind the cell  29  with liquid sample  30  is used to measure the intensity of excitation light passed through the liquid sample  30  to evaluate it&#39;s optical density. A lens  40  serves to focus the collimated excitation light beam onto the absorption photo-detector  9  active area. The absorption photo-detector  9  is preferably a photodiode. 
     Characteristic feature of the first embodiment of the device lie in the presence of the means for self-calibration of wavelength scales of both monochromators shown in  FIGS. 3 and 4 .  FIG. 3  shows a partial sectional view generally taken along the line A-A of  FIG. 2 . A wavelength calibration photo-detector  7  (e.g. a photodiode) is located behind the (additional) third exit slit  43  of the excitation monochromator; the third exit slit  43  being located in the locus of the partly reflected from the beamsplitter&#39;s  20  facing the grating  22  side and focused by the grating “zero-order” spectrum (i.e. the spectral order which contains all wavelengths of light reflected by the grating). The wavelength calibration photo-detector  7  detects a signal maximum at the grating angular position wherein the grating normal at its vertex coincides with the optical axis of incident light beam on the grating. At this grating angular position light with a known wavelength determined by the grating constant and the beam deviation angle (angle between straight lines connecting the entrance slit and exit slit centers with the grating vertex) is passing through the first or the second exit slit,  25  and  26  respectively. Microcontroller  14  compares periodically and after each switching on the actual wavelength calibration photo-detector  7  signal maximum position with the preadjusted wavelength scale (e.g. an encoder) connected to the grating drive. If a wavelength scale error is detected, the microcontroller  14  recalibrates the scale. 
     Wavelength self-calibration means of the emission monochromator are illustrated in the  FIGS. 2 and 4 : a wavelength calibration light source  12  is located at the (additional) third entrance slit  44  of the emission monochromator (see  FIG. 4 ); a diaphragm  45  serves for restricting the beam divergence; a beam inclining mirror  41  bends the light beam into the meridional plane of the diffraction grating  37  and directs the slightly diverging beam to the grating center (see  FIG. 2 ). Angle a between the central incident rays from the calibration light source  12  and from the first or the second entrance slit,  33  and  35  respectively, is equal to the emission monochromator deviation angle β. Thus at the grating  37  angular position wherein the grating normal at its vertex passes through the entrance slit  35  center the photo-detector  13  detects “zero-order” signal maximum from the wavelength calibration light source  12 . The light source  12  is switched on by the microcontroller  14  at the time of checking the wavelength scale calibration. Microcontroller  14  compares periodically and after each switching on the actual signal maximum position with the preadjusted wavelength scale (e.g. an encoder) connected to the grating drive. If a wavelength scale error is detected, the microcontroller  14  recalibrates the scale. Angles α and β are set equal in this embodiment only for simplification of preadjustment procedures, principally the angle α may have any other value, different from the value of angle β. 
     The wavelength calibration light source  12  is an ordinary light emitting diode (LED); there are no requirements for its spectral characterization as it works in so called “zero-order” spectrum. 
     A reference photo-detector  6  (see  FIG. 3 ) is used to measure the variations of intensity of light passed through the excitation monochromator entrance slit  19  for a fluorescence spectra data acquisition procedure performed by the microcontroller  14 . The diverging light beam from the entrance slit  19  is partly reflected from the beamsplitter&#39;s  20  facing the slit  19  side and focused by the lens  42  onto the active area of photo-detector  6 . Photo-detector  6  signal amplitude may be also used for diagnostics of light source  1  ageing. As an option the ratio of the amplitudes of signals from the wavelength calibration photo-detector  7  and the reference photo-detector  6  may be used for diagnostics of the state of the diffraction grating  22  which reflectance may decrease due to contamination of its active area in case of working in harsh environmental conditions. 
     The second embodiment of the optical layout, which may be located within the first embodiment, having means for measuring dense samples is shown in  FIG. 5 . This layout is identical to the first preferred embodiment illustrated in  FIG. 2  with the exception of changed configuration of the optical cell assembly consisting of a right angle prism  46 , a dense sample container  47 , a dense sample  48 , a transparent cover  49 , and a right angle prism  50  (see  FIGS. 5-8 ); also this layout does not contain means for measuring absorption spectra (focusing lens  40  and absorption photo-detector  9  shown in  FIG. 2 ). Outgoing through the exit slit  25  (see  FIG. 5 ), a diverging light beam is collimated by the lens  28  and bent by the right angle prism  46  slantwise downward onto the dense sample  48  located in a cavity of the sample container  47  and covered by the transparent cover  49  (see  FIGS. 6-7 ). By adjusting the angular position of the right angle prism  46  around the optical axis of the light beam incident to the prism the angle of incidence γ to the sample cover  49  may be adjusted to a necessary value, generally about 45°. A fluorescence light beam emitted by the sample  48  in the normal direction is bent by means of the right angle prism  50  (see  FIG. 8 ) by 90° and focused by the lens  32  (see  FIG. 5 ) onto the entrance slit  33  of the emission monochromator. 
     The identity of the basic parts of the first and the second preferred embodiments of the optical layout enables the construction of these two embodiments jointly in the same device having two different interchangeable optical cell assemblies; the first assembly containing the cell  29  for dispose of a liquid sample  30  and the right angle prism  31  (see  FIG. 2 ), the second assembly containing the right angle prism  46 , the sample container  47  for dispose of a dense sample  48 , the transparent cover  49 , and a right angle prism  50  (see  FIGS. 5-8 ). In an alternative construction of the device realizing the both embodiments, the right angle prisms  31  and  50  may be excluded from the respective interchangeable cell assembly and substituted by turnable by 90° around the axis  53  passing through the lens  32  and slit  33  (see  FIGS. 2 and 5 ) centers a single right angle prism added to the main device. 
     Alternatively and as an option the beam-inclining mirror  24  may be performed as a switching mirror turnable around the axis  51  to remove the mirror from the light path and enable the light beam to exit from the monochromator through an optional second exit slit  26  to an optional optical fiber connector  27  ( FIG. 2 ). 
     As an option the beam-inclining mirror  34  may be performed as a switching mirror turnable around the axis  52  to remove the mirror from the light path and enable the alternative light beam to enter into the monochromator from an optional optical fiber connector  36  through an optional second entrance slit  35  of the emission monochromator ( FIG. 2 ). 
     Optical fiber connectors  27  and  36  serve as an option for connection of an alternative external sample measuring device—e.g. a fiber optic immersion fluorescence probe (not described in the present patent application). 
     The data processing: detection, recognition, quantification, displaying and transfer may be performed by an integrated or an external computer system. A standard pocket PC or any other computer system can be integrated into the device, which would be an internal PC. Alternatively, the processing could be done by a separate unit in a pocket or on the table, which would be an external PC. In the laboratory it is probably more convenient to operate with desktop PC. On site, a pocket PC (integrated or hand-held) is preferable. 
     In a further embodiment, the method of this invention includes the steps of: 
     1. Sample preparation: Sampling of a sample and a special sample preparation using tools and kits or automated preparation. If direct measurements are suitable (e.g. for solid or powder samples), this stage may be omitted. Such samples may be introduced into the device by using cell assembly for dense samples. 
     If a sample requires pre-treatment, the following steps are performed (manually or automatically). The samples for analysis are taken manually by sampling tool (tube or tweezers depending on sample form). A 3 mg of powder or crushed pill that is taken by volumetric tube is dissolved in 150 ml of distilled water in a cup. The water with powder is mixed to complete dilution of the powder in water. 
     A small amount of dried plant that is taken by tweezers is put into 60 ml of distilled water (or other solvent) in cup and mixed. Then the sample must be filtered The samples can be placed or injected into the active cell of the device manually or automatically accordingly. 
     Pushing the adequate button (for example, “Cocaine hydrochloride”, or “Cocaine base”, or “Ecstasy”, or “Marijuana”, etc.) will be followed by automatic SFS measurements of the sample in the proper measuring conditions. 
     2. Detection and quantification: Measurements should be done in the specific spectral area to shorten the necessary measurement time and to decrease fluorescence background influence. Measurements have to be done with the appropriate accumulation time and amplification. 
     Fluorescence measurements of the 3D data (Excitation, Emission, Intensity) may be provided with parallel photometric measurements to control optical density of the liquid sample. (The data related to optical density of the sample are used for proper detection and quantification of the complex substance mixtures). 
     The data processing: detection, recognition, quantification, displaying and transfer may be performed by an integrated or an external computer system. The expert system detects and quantifies substances of interest automatically. Analysis uses the spectral database with and preliminary compiled calibrated libraries, multivariate calibrations and Neural Nets to solve any kind of the complex detection and quantification problem. 
     3. Results of measurements: Results should be indicated as text and numbers such as a name of a detected substance of interest and, if it is predetermined, as a concentration number. Concentration may be expressed in weight per volume units or as a percentage from the total sample. 
     4. Data storage: results have to be automatically stored into the device memory and possibly transferred to a remote different official site as the personal and sample data with the measured raw spectral data, their proper parameters and with the results of detection (quantification) and the date and time of analysis. 
     An external processing means, such as a PC, a notebook, hand-held etc. is used for database store and final analysis 
     According to different kinds of street drug samples their preparation for measurements may be done using special kit of containers with necessary solvents in predetermined volume or without kit directly into device measuring cell. 
     Measurements may be done for all forms of samples (powder or solid, or liquid) directly or after automatic preparation. The sample inputted into device may be automatically weighed to calculate measuring data in percents or in concentrations related to the weight of the sample. It may be also automatically diluted according to the device photometric measurements and software algorithm. Each way is predetermined regarding the giving drug or group of drugs analysis. 
     If the method does not require measurements of liquid form of the sample, the last may be measured outside the device or inside it from the surface of the sample. To provide the method with reliable and simplified liquid sample preparation device may be supplied with sampling tools and special kits: sampling tool for approximate 3 mg of the sample, disposable containers with solvents and a cartridge (holder) to put the container into device for measurements. Preparation of the sample may be done in automatic mode using outer or inner means. 
     The preparation of the sample can be done in automatic mode using outer means, which is an automatic sampler with dilution, washing and mixing functions. The preparation of the sample can also be done in automatic mode using inner means, which could be a sample preparation panel with dilution, washing and mixing functions. 
     Personal data of the suspect and a short title for the sample with the date of analysis may be initially entered into device memory using its keyboard. 
     The device provides SFS detection and quantification of the substances of interest in the range 5-100% of the sample taken for analysis. All data are stored and available as spectra with parameters of their measurements and date. 
     EXAMPLE 1 
     Detection of Cocaine in experimental samples: Experimental samples were prepared based upon known common ingredients of Cocaine street samples and their ratio (information from experts and literature): Cocaine hydrochloride; Lidocaine or Caffeine, or Procaine (as adulterants) and Glucose or Lactose, or Baking soda, or Corn Starch (as diluents) with Cocaine presence from 100% to 5%. 3 mg of the following samples dissolved in water, diluted 1:150 and measured for Cocaine detection (see Table 1 below for results): 
     
       
         
               
             
               
               
               
             
               
               
               
             
           
               
                 TABLE 1 
               
             
             
               
                   
               
               
                 Results of Cocaine detection in experimental samples. 
               
             
          
           
               
                 Samples 
                 Composition 
                 Results 
               
               
                   
               
             
          
           
               
                 1 
                 caf85%_co5% 
                 Yes 
               
               
                 2. 
                 caf100% 
                 No 
               
               
                 3 
                 caf100% 
                 No 
               
               
                 4 
                 co85%_caf5%_g10% 
                 Yes 
               
               
                 5 
                 co85%_caf5%_l10% 
                 Yes 
               
               
                 6 
                 co85%_caf5%_s10% 
                 Yes 
               
               
                 7 
                 co85%_lid5%_g10% 
                 Yes 
               
               
                 8 
                 co85%_lid5%_l10% 
                 Yes 
               
               
                 9 
                 co85%_caf5%_g5% 
                 Yes 
               
               
                 10 
                 co85%_caf5%_l10% 
                 Yes 
               
               
                 11 
                 co85%_caf5%_s10% 
                 Yes 
               
               
                 12 
                 co85%_caf5%_st10% 
                 Yes 
               
               
                 13 
                 co85%_lid5%_g10% 
                 Yes 
               
               
                 14 
                 co85%_lid5%_g10% 
                 Yes 
               
               
                 15 
                 co85%_lid5%_l10% 
                 Yes 
               
               
                 16 
                 co85%_lid5%_s10% 
                 Yes 
               
               
                 17 
                 co85%_lid5%_st10% 
                 Yes 
               
               
                 18 
                 co85%_lid3_0204a.dat 
                 Yes 
               
               
                 19 
                 co85%_lid3_0304a.dat 
                 Yes 
               
               
                 20 
                 co85%_prc5%_g10% 
                 Yes 
               
               
                 21 
                 co85%_prc5%_l10% 
                 Yes 
               
               
                 22 
                 co85%_prc5%_s10% 
                 Yes 
               
               
                 23 
                 co85%_prc5%_st10% 
                 Yes 
               
               
                 24 
                 co85%_prc15% 
                 Yes 
               
               
                 25 
                 co85%_prc15% 
                 Yes 
               
               
                 26 
                 co85%_prc5%_g10% 
                 Yes 
               
               
                 27 
                 co85%_prc5%_l10% 
                 Yes 
               
               
                 28 
                 co85%_prc5%_st10% 
                 Yes 
               
               
                 29 
                 co90%_g10% 
                 Yes 
               
               
                 30 
                 co90%_l10% 
                 Yes 
               
               
                 31 
                 co90%_s10% 
                 Yes 
               
               
                 32 
                 co90%_st10% 
                 Yes 
               
               
                 33 
                 co95%_caf5% 
                 Yes 
               
               
                 34 
                 co95%_caf5% 
                 Yes 
               
               
                 35 
                 co95%_lid5% 
                 Yes 
               
               
                 36 
                 co95%_lid5% 
                 Yes 
               
               
                 37 
                 co95%_prc5% 
                 Yes 
               
               
                 38 
                 co95%_prc5% 
                 Yes 
               
               
                 39 
                 co100% 
                 Yes 
               
               
                 40 
                 g100% 
                 No 
               
               
                 41 
                 l5%_co95% 
                 Yes 
               
               
                 42 
                 l100% 
                 No 
               
               
                 43 
                 lid100% 
                 No 
               
               
                 44 
                 prc15%_co85% 
                 Yes 
               
               
                 45 
                 prc20%_co80% 
                 Yes 
               
               
                 46 
                 prc100% 
                 No 
               
               
                 47 
                 prc100% 
                 No 
               
               
                 48 
                 prc100% 
                 No 
               
               
                 49 
                 s100% 
                 No 
               
               
                 50 
                 st95%_co5% 
                 Yes 
               
               
                 51 
                 st100% 
                 No 
               
               
                   
               
               
                 Samples Definitions: 
               
               
                 co—Cocaine; 
               
               
                 caf—Caffeine; 
               
               
                 lid—Lidocaine; 
               
               
                 prc—Procaine; 
               
               
                 g—Glucose; 
               
               
                 l—Lactose; 
               
               
                 s—Baking Soda; 
               
               
                 st—Corn Starch. 
               
             
          
         
       
     
     Detection and quantification of Cocaine in experimental samples: Experimental samples were prepared based upon known common ingredients of Cocaine street samples and their ratio (information from experts and literature): Cocaine hydrochloride; Lidocaine or Caffeine, or Procaine (as adulterants) and Glucose or Lactose, or Baking soda, or Corn Starch (as diluents). Cocaine presence in the range from 85% up to 100%. 
     3 mg of the samples were dissolved in water, diluted 1:150 and measured for Cocaine quantification (see Table 2 below for results): 
     
       
         
               
             
               
               
               
               
             
               
               
               
               
             
           
               
                 TABLE 2 
               
             
             
               
                   
               
               
                 Results of Cocaine detection and quantification in experimental samples. 
               
             
          
           
               
                 Samples 
                 Composition 
                 Results 
                 Error, % 
               
               
                   
               
             
          
           
               
                 1 
                 caf100% 
                   
                   
               
               
                 2 
                 co85%_caf5%_g10% 
                 Cocaine 84.7% 
                 0.4 
               
               
                 3 
                 co85%_caf5%_l10% 
                 Cocaine 83.7% 
                 1.5 
               
               
                 4 
                 co85%_caf5%_s10% 
                 Cocaine 85.6% 
                 0.7 
               
               
                 5 
                 co85%_caf5%_st10% 
                 Cocaine 84.8% 
                 1.1 
               
               
                 6 
                 co85%_lid5%_g10% 
                 Cocaine 82.6% 
                 2.8 
               
               
                 7 
                 co85%_lid5%_l10% 
                 Cocaine 85.1% 
                 0.1 
               
               
                 8 
                 co85%_lid5%_s10% 
                 Cocaine 87.7% 
                 3.2 
               
               
                 9 
                 co85%_lid5%_st10% 
                 Cocaine 88.1% 
                 3.7 
               
               
                 10 
                 co85%_lid15% 
                 Cocaine 81.3% 
                 4.3 
               
               
                 11 
                 co85%_lid15% 
                 Cocaine 81.5% 
                 4.1 
               
               
                 12 
                 co85%_prc15% 
                 Cocaine 85.4% 
                 0.5 
               
               
                 13 
                 co85%_prc5%_g10% 
                 Cocaine 87.4% 
                 2.9 
               
               
                 14 
                 co85%_prc5%_l10% 
                 Cocaine 85.8% 
                 1.1 
               
               
                 15 
                 co85%_prc5%_s10% 
                 Cocaine 83.9% 
                 1.3 
               
               
                 16 
                 co85%_prc5%_st10% 
                 Cocaine 82.7% 
                 2.7 
               
               
                 17 
                 co100% 
                 Cocaine 95.4% 
                 4.6 
               
               
                 18 
                 g100% 
               
               
                 19 
                 l100% 
               
               
                 20 
                 lid100% 
               
               
                 21 
                 prc100% 
               
               
                 22 
                 prc100% 
               
               
                 23 
                 s100% 
               
               
                 24 
                 st100% 
               
               
                   
               
               
                 Samples Definitions: 
               
               
                 co—Cocaine; 
               
               
                 caf—Caffeine; 
               
               
                 lid—Lidocaine; 
               
               
                 prc—Procaine; 
               
               
                 g—Glucose; 
               
               
                 l—Lactose; 
               
               
                 s—Baking Soda; 
               
               
                 st—Corn Starch. 
               
             
          
         
       
     
     EXAMPLE 2 
     Detection of Marijuana in experimental samples: Experimental samples were prepared based upon known common ingredient of street samples of Marijuana (information from experts and literature): 
     Marijuana 5% plus tobacco 95% 
     Marijuana 30% plus tobacco 70% 
     Marijuana 50% plus tobacco 50% 
     Marijuana 70% plus tobacco 30% 
     Marijuana 100% 
     Tobacco 100% (as zero point). 
     Tobacco was taken from Canadian cigarettes: du Maurier Light®; du Maurier Extra Light® and Belmont Milds®, and USA cigarettes: Marlboro®; Camel®; Winstont®; Salem® and Kool®. 
     3-6 mg of Marijuana were mixed with 3-6 ml of Ethanol, diluted 1:10 and measured for Marijuana detection (see Table 1 below for results of detection). 
     
       
         
               
             
               
               
               
             
               
               
               
             
           
               
                 TABLE 1 
               
             
             
               
                   
               
               
                 Results of Marijuana detection in experimental samples. 
               
             
          
           
               
                 Samples 
                 Composition 
                 Results 
               
               
                   
               
             
          
           
               
                 1 
                 blmnt100% 
                 No 
               
               
                 2 
                 blmnt100% 
                 No 
               
               
                 3 
                 blmnt100% 
                 No 
               
               
                 4 
                 camel100% 
                 No 
               
               
                 5 
                 kool100% 
                 No 
               
               
                 6 
                 mj5%_camel95% 
                 Yes 
               
               
                 7 
                 mj5%_kool95% 
                 Yes 
               
               
                 8 
                 mj5%_mrlbr95% 
                 Yes 
               
               
                 9 
                 mj5%_salem95% 
                 Yes 
               
               
                 10 
                 mj5%_wnstn95% 
                 Yes 
               
               
                 11 
                 mj10%_salem90% 
                 Yes 
               
               
                 12 
                 mj10%_wnstn90% 
                 Yes 
               
               
                 13 
                 mj15%_mrlbr85% 
                 Yes 
               
               
                 14 
                 mj15%_salem85% 
                 Yes 
               
               
                 15 
                 mj30%_blmnt70% 
                 Yes 
               
               
                 16 
                 mj30%_camel70% 
                 Yes 
               
               
                 17 
                 mj30%_kool70% 
                 Yes 
               
               
                 18 
                 mj30%_mrlbr70% 
                 Yes 
               
               
                 19 
                 mj30%_salem70% 
                 Yes 
               
               
                 20 
                 mj30%_wnstn70% 
                 Yes 
               
               
                 21 
                 mj50%_blmnt50% 
                 Yes 
               
               
                 22 
                 mj50%_blmnt50% 
                 Yes 
               
               
                 23 
                 mj50%_mrel50% 
                 Yes 
               
               
                 24 
                 mj50%_mrl50% 
                 Yes 
               
               
                 25 
                 mj50%_camel50% 
                 Yes 
               
               
                 26 
                 mj50%_kool50% 
                 Yes 
               
               
                 27 
                 mj50%_salem50% 
                 Yes 
               
               
                 28 
                 mj50%_wnstn50% 
                 Yes 
               
               
                 29 
                 mj70%_blmnt30% 
                 Yes 
               
               
                 30 
                 mj70%_camel30% 
                 Yes 
               
               
                 31 
                 mj70%_kool30% 
                 Yes 
               
               
                 32 
                 mj70%_mrlbr30% 
                 Yes 
               
               
                 33 
                 mj70%_salem30% 
                 Yes 
               
               
                 34 
                 mj70%_wnstn30% 
                 Yes 
               
               
                 35 
                 mj100% 
                 Yes 
               
               
                 36 
                 mj100% 
                 Yes 
               
               
                 37 
                 mj100% 
                 Yes 
               
               
                 38 
                 mrel100% 
                 No 
               
               
                 39 
                 mrl100% 
                 No 
               
               
                 40 
                 mrlbr100% 
                 No 
               
               
                 41 
                 salem100% 
                 No 
               
               
                 42 
                 wnstn100% 
                 No 
               
               
                   
               
               
                 Samples Definitions: 
               
               
                 mj—Marijuana; 
               
               
                 blmnt—Belmont Milds ®; 
               
               
                 camel—Camel ®; 
               
               
                 kool—Kool ®; 
               
               
                 mre—du Maurier Light ®; 
               
               
                 mrel—du Maurier Extra Light ®; 
               
               
                 mrlbr—Marlboro ®; 
               
               
                 salem—Salem ®; 
               
               
                 wnstn—Winston ®.