bluuebunny/crossref_metadata_2025 huggingface dataset:
Differential Pulse Polarographic Determination of Lead in Complex Materials after Adsorption of Its N-Methylethylxanthocarbamate Complex on Microcrystalline Naphthalene or on NMethylethylxanthocarbamate–Benzyldimethyltetradecylammonium–Naphthalene Adsorbent
Authors: Hussain Mohammad Farid , Sangahi Anil Kumar , Ahmad Iqbal , Puri Bal Krishan
Published: February 2020

Lead is quantitatively adsorbed as the lead N-methylethylxanthocarbamate (MEXC)–benzyldimethyltetradecylammonium (BDTA) ion pair complex on microcrystalline naphthalene in the pH range 4.0–11.0. The metal is desorbed with HCl and determined by differential pulse polarography. Alternatively lead can be quantitatively adsorbed on the adsorbent (MEXC–BDTA–naphthalene) packed in a column at a flow rate of 1–2 mL/min and determined similarly. Dissolved oxygen is removed by adding a few milliliters of 4% NaBH4 solution. The detection limit is 0.12 μg/mL at the minimum instrumental settings (signal-to-noise ratio, 2). Linearity was obtained over the concentration range 0.3–20.0 μg/mL with a correlation factor of 0.9998 and a relative standard deviation of ± 0.98%. Various parameters, such as the effect of pH, volume of aqueous phase, flow rate, and the interference of a large number of metal ions and anions, were studied in detail to optimize the conditions for the trace determination of lead in various standard alloys, standard biological materials, and environmental samples.
Preparation of Samples for Gas Chromatography/Mass Spectrometry Analysis of Phthalate and Adipate Esters in Plasma and Beverages by Steam Distillation and Extraction
Authors: Kato Kayoko , Yoshimura Yoshihiro , Nakazawa Hiroyuki , Ito Yuko , Oka Hisao
Published: February 2020

Phthalate and adipate esters are present in relatively large amounts in the environment, resulting in their large blank values at analysis and making precise analysis difficult. We developed a highly sensitive analytical method for phthalate and adipate esters in plasma and beverages by lowering the blank values that interfere with analysis. The method uses a closed distillation cleanup system in which steam distillation and extraction are performed simultaneously. The recoveries from beverages and plasma were both satisfactory, ranging from 90.2 to 118.3%, relative standard deviation (RSD) = 2.8–5.3%, and 96.2–134.4%, RSD = 2.2–6.5%, respectively. The detection limits of dibutyl phthalate and di-2-ethyl hexyl phthalate were 5 ng/mL, and those of diethyl phthalate, butyl benzyl phthalate, and di-2-ethyl hexyl adipate were 10 ng/mL in rabbit plasma and beverages.
Detection Methods and Performance Criteria for Genetically Modified Organisms
Authors: Bertheau Yves , Diolez Annick , Kobilinsky André , Magin Kimberly
Published: February 2020

Detection methods for genetically modified organisms (GMOs) are necessary for many applications, from seed purity assessment to compliance of food labeling in several countries. Numerous analytical methods are currently used or under development to support these needs. The currently used methods are bioassays and protein- and DNA-based detection protocols. To avoid discrepancy of results between such largely different methods and, for instance, the potential resulting legal actions, compatibility of the methods is urgently needed. Performance criteria of methods allow evaluation against a common standard. The more-common performance criteria for detection methods are precision, accuracy, sensitivity, and specificity, which together specifically address other terms used to describe the performance of a method, such as applicability, selectivity, calibration, trueness, precision, recovery, operating range, limit of quantitation, limit of detection, and ruggedness. Performance criteria should provide objective tools to accept or reject specific methods, to validate them, to ensure compatibility between validated methods, and be used on a routine basis to reject data outside an acceptable range of variability. When selecting a method of detection, it is also important to consider its applicability, its field of applications, and its limitations, by including factors such as its ability to detect the target analyte in a given matrix, the duration of the analyses, its cost effectiveness, and the necessary sample sizes for testing. Thus, the current GMO detection methods should be evaluated against a common set of performance criteria.
Validation Studies and Proficiency Testing
Authors: Anklam Elke , Heinze Petra , Kay Simon , Eede Guy van den , Popping Bert
Published: February 2020

Genetically modified organisms (GMOs) entered the European food market in 1996. Current legislation demands the labeling of food products if they contain <1% GMO, as assessed for each ingredient of the product. To create confidence in the testing methods and to complement enforcement requirements, there is an urgent need for internationally validated methods, which could serve as reference methods. To date, several methods have been submitted to validation trials at an international level; approaches now exist that can be used in different circumstances and for different food matrixes. Moreover, the requirement for the formal validation of methods is clearly accepted; several national and international bodies are active in organizing studies. Further validation studies, especially on the quantitative polymerase chain reaction methods, need to be performed to cover the rising demand for new extraction methods and other background matrixes, as well as for novel GMO constructs.
Predictions for Rapid Methods and Automation in Food Microbiology
Authors: Fung Daniel Y C
Published: February 2020

A discussion is presented on the present status of rapid methods and automation in microbiology. Predictions are also presented for development in the following areas: viable cell counts; real-time monitoring of hygiene; polymerase chain reaction, ribotyping, and genetic tests in food laboratories; automated enzyme-linked immunosorbent assay and immunotests; rapid dipstick technology; biosensors for Hazard Analysis Critical Control Point programs; instant detection of target pathogens by computer-generated matrix; effective separation and concentration for rapid identification of target cells; microbiological alert systems in food packages; and rapid alert kits for detecting pathogens at home.
Simultaneous Determination of Estradiol and Medroxyprogesterone Acetate in Pharmaceutical Formulations by Second-Derivative Spectrophotometry
Authors: Toral M Inés , Soto César , Richter Pablo , Tapai Ana E
Published: February 2020

This paper reports a simple and fast method for the simultaneous determination of estradiol (ED) and medroxyprogesterone acetate (MP) in pharmaceutical formulations by second-derivative spectrophotometry. Methanol was used to extract the drugs from formulations, and subsequently the extracts were evaluated directly by derivative spectrophotometry. The drugs were determined simultaneously by using the graphic method at 297.4 nm for ED and the zero-crossing method at 273.4 nm for MP. If both compounds are present together in a sample, it is possible to quantitate one in the presence of the other. The best signal-to-noise ratio was found when the second derivative of the spectrum was used. The linear ranges for determination of the drugs were 4.7 × 10−6 to 1.6 × 10−4 and 7.2 × 10−6 to 2.0 × 10−4 mol/L for ED and MP, respectively. The ingredients commonly found in commercial pharmaceutical formulations do not interfere with the determination. Chemical and spectral variables were optimized for the determination of both analytes. Good levels of repeatability (relative standard deviation), 1.4 and 1.9%, were obtained for ED and MP, respectively. The proposed method was applied to the determination of these drugs in pharmaceutical formulations.
French Laboratory Proficiency Testing Program for Food Microbiology
Authors: Augustin Jean-Christophe , Carlier Vincent
Published: February 2020

The proficiency testing program in food microbiology (Réseau d' Analyses et d'Echanges en Microbiologie des Aliments; RAEMA), created in 1988, currently includes 440 participating laboratories. The program establishes proficiency in detection of Salmonella and Listeria monocytogenes, as well as quantitation of aerobic microorganisms, Enterobacteriaceae, coliforms, Escherichia coli, Clostridium perfringens, coagulase-positive Staphylococcus, and Listeria monocytogenes. Twice a year, 5 test samples are sent to participants to assess their precision and trueness for enumeration and detection of microorganisms. Results show an increasing involvement of food microbiology laboratories in quality assurance programs and use of standard and validated analytical methods. However, the percentage of laboratories obtaining questionable and unsatisfactory microbiological results remains relatively onstant.
Determination of Brevetoxins in Shellfish by the Neuroblastoma Assay
Authors: Truman Penelope , Stirling David J , Northcote Peter , Lake Robin J , Seamer Catherine , Hannah Donald J
Published: February 2020

A neuroblastoma assay for determination of brevetoxins in shellfish was developed together with a method for sample cleanup that allows separation of brevetoxins from most of the components that cause matrix interference in the assay. This improved assay method was applied to a range of shellfish samples with different characteristics. Extracts of naturally contaminated and nontoxic shellfish together with extracts spiked with known amounts of toxin were tested. The results demonstrated that brevetoxins could be reliably detected in shellfish extracts at concentrations below the regulatory limit. Brevetoxin activity was detected in 15 of 23 samples from 5 separate toxicity incidents in which shellfish tested positive in the neurotoxic shellfish poisoning (NSP) mouse bioassay. Twelve of these positive NSP results came from 2 toxicity incidents. Yessotoxin was the major contributor to toxicity in 2 other incidents, although some samples contained both yessotoxin and brevetoxin. The sample from the remaining incident contained an unidentified toxin bioactivity, together with gymnodimine. In contrast to earlier versions of the neuroblastoma assay, gymnodimine was not detected by this modified method.
Novel Reference Molecules for Quantitation of Genetically Modified Maize and Soybean
Authors: Kuribara Hideo , Shindo Yoichiro , Matsuoka Takeshi , Takubo Ken , Futo Satoshi , Aoki Nobutaro , Hirao Takashi , Akiyama Hiroshi , Goda Yukihiro , Toyada Masatake , Hino Akihiro
Published: February 2020

New quantitation methods based on a real-time polymerase chain reaction (PCR) technique were developed for 5 lines of genetically modified (GM) maize, including MON810, Event176, Bt11, T25, and GA21, and a GM soy, Roundup Ready. Oligonucleotide DNA, including specific primers and fluorescent dye, labeled probes, were designed for PCRs. Two plasmids were constructed as reference molecules (RMs) for the detection of GM maize and GM soy. The molecules contain the DNA sequences of a specific region found in each GM line, universal sequences used in various GM lines, such as cauliflower mosaic virus 35S promoter and nopaline synthase terminator, and the endogenous DNA sequences of maize or soy. By using these plasmids, no GM maize and GM soy were required as reference materials for the qualitative and quantitative PCR technique. Test samples containing 0, 0.10, 0.50, 1.0, 5.0, and 10% GM maize or GM soy were quantitated. At the 5.0%level, the bias (mean–true value) ranged from 2.8 to 19.4% and the relative standard deviation was <5.2%. These results show that our method involving the use of these plasmids as RMs is reliable and practical for quantitation of GM maize and GM soy.
Temperature-Sensitive Resolution of cis- and trans-Fatty Acid Isomers of Partially Hydrogenated Vegetable Oils on SP-2560 and CP-Sil 88 Capillary Columns
Authors: Ratnayake W M Nimal , Plouffe Louise J , Pasquier Elodie , Gagnon Claude
Published: February 2020

This study examines the effect of the column operating temperature of 100 m SP-2560 and CP-Sil 88 capillary gas chromatographic (GC) columns on the separation of cis- and trans-octadecenoic (18:1) isomers in partially hydrogenated vegetable oils. The overlapping GC peaks were measured at column isothermal temperatures of 170, 175, 180, 185, and 190°C. With both columns, isothermal operation at 180°C produced the fewest overlapping peaks of the cis and trans isomers. At this temperature, all trans-18:1 isomers, except 13t-18:1 (t = trans), 14t-18:1, and 15t-18:1 isomers were resolved from 14t-18:1, the cis-18:1 isomers. The peaks of the 13t-18:1 and 14t-18:1 isomer pair, which always elute together, overlapped peaks of the 6c-18:1 (c = cis), 7c-18:1, and 8c-18:1 isomers; the peak of the 15t-18:1 isomer overlapped the major cis-18:1 peak, which was mainly due to 9c-18:1. Isothermal operations above or below 180°C produced some additional overlapping problems. At 185 and 190°C, the peaks of the 16t-18:1 and 13c-18:1 isomers overlapped. At 175 and 170°C, the 16t-18:1 peak overlapped the 14c-18:1 peak, and the peaks of the 13t + 14t-18:1 isomer pair partially overlapped the major cis-18:1 peak. The separation of 11c-20:1 and α-linolenic acid and its geometric isomers was also affected by the column operating temperature. Isothermal operation of the SP-2560 column at 180°C produced a baseline separation of 11c-20:1 and α-linolenic acid and its geometric isomers, whereas with the CP-Sil 88 column the best resolution was obtained at 170°C. The results of this study show that the SP-2560 capillary column has a slight advantage over the CP-Sil 88 column for the simultaneous resolution of all the fatty acids generally found in partially hydrogenated vegetable oils.
Validation of Real-Time PCR Analyses for Line-Specific Quantitation of Genetically Modified Maize and Soybean UsingNew Reference Molecules
Authors: Shindo Yoichiro , Kuribara Hideo , Matsuoka Takeshi , Futo Satoshi , Sawada Chihiro , Shono Jinji , Akiyama Hiroshi , Goda Yukihiro , Toyoda Masatake , Hino Akihiro ,   Collaborators:, Asano T , Hiramoto M , Iwaya A , Jeong S I , Kajiyama N , Kato H , Katsumoto H , Kim Y M , Kwak H S , Ogawa M , Onozuka Y , Takubo K , Yamakawa H , Yamazaki F , Yoshida A , Yoshimura T
Published: February 2020

Novel analytical methods based on real-time quantitative polymerase chain reactions by use of new reference molecules were validated in interlaboratory studies for the quantitation of genetically modified (GM) maize and soy. More than 13 laboratories from Japan, Korea, and the United States participated in the studies. The interlaboratory studies included 2 separate stages: (1) measurement tests of coefficient values, the ratio of recombinant DNA (r-DNA) sequence, and endogenous DNA sequence in the seeds of GM maize and GM soy; and (2) blind tests with 6 pairs of maize and soy samples, including different levels of GM maize or GM soy. Test results showed that the methods are applicable to the specific quantitation of the 5 lines of GM maize and one line of GM soy. After statistical treatment to remove outliers, the repeatability and reproducibility of these methods at a level of 5.0% were <13.7 and 15.9%, respectively. The quantitation limits of the methods were 0.50% for Bt11, T25, and MON810, and 0.10% for GA21, Event176, and Roundup Ready soy. The results of blind tests showed that the numerical information obtained from these methods will contribute to practical analyses for labeling systems of GM crops.
Rapid Method for Trace Determination of Organochlorine Pesticides and Polychlorinated Biphenyls in Yogurt
Authors: Yagüe Cristina , Herrera Antonio , Ariño Agustín , Lázaro Regina , Bayarri Susana , Conchello Pilar
Published: February 2020

A new multiresidue method was developed for the analysis of 19 organochlorine pesticides and 6 polychlorinated biphenyls in yogurt. The sample was extracted twice with acetone by homogenization with an Ultra-Turrax dispersing unit, and the combined extracts were filtered. The extract was then purified by reversed-phase C18 columns and subjected to further cleanup with neutral alumina columns. The residues were determined by gas chromatography with electron capture detection. After the method was optimized, it was validated by determination of recovery percentages, precision (repeatability and reproducibility), and sensitivity (detection and quantitation limits) with yogurt samples fortified at 10 and 1 μg/kg concentration levels. The recovery of 23 organochlorine residues ranged from 77 to 95% at a level of 10 μg/kg, from 74 to 102% at a level of 1 μg/kg, and between 54 and 61% for dieldrin and α-endosulfan. The method is repeatable and reproducible, with relative standard deviation values <19% for all residues except dieldrin. Detection and quantitation limits were between 0.02 and 0.62 μg/kg. The analytical method proposed was quick, accurate, repeatable, and reproducible for the determination of organochlorine residues in yogurt samples.
Determination of Phosphorus in Fertilizers by Inductively Coupled Plasma Atomic Emission Spectrometry
Authors: Yang Wei Min , Boles Rhonda L , Mawhinney Thomas P
Published: February 2020

An inductively coupled plasma atomic emission spectrometry (ICP-AES) method was developed for the determination of phosphorus in fertilizers. Total phosphorus, direct extraction available phosphorus (EDTA), and water-soluble phosphorus, reported as phosphorus pentoxide (P2O5), in 15 Magruder check fertilizers were measured by ICP-AES, and the results were compared with those obtained by the AOAC official method. Five analytical wavelengths of phosphorus, 177.499, 178.287, 213.618, 214.914, and 253.565 nm, were tested for the determination of phosphorus in fertilizers, and their detection limits were obtained. Acid effects of perchloric acid and possible matrix effects of aluminum, calcium, magnesium, potassium, and sodium were negligible for phosphorus determination. Wavelength 213.618 nm was the best analytical wavelength for phosphorus determination by all 3 sample preparation methods for the selected Magruder fertilizers. The results demonstrated that the accuracy and precision of the ICP-AES method were comparable with those of the official methods.
Sequential Determination of Salicylic and Acetylsalicylic Acids by Amperometric Multisite Detection Flow Injection Analysis
Authors: Catarino Rita I L , Garcia M Beatriz Q , Lapa Rui A S , Lima José L F C , Barrado Enrique
Published: February 2020

An amperometric multisite detection flow injection analysis (FIA) system was developed for sequential determination of 2 analytes with a single sample injection and single detector. Tubular composite carbon electrodes with an inner diameter similar to that of the FIA manifold tubing were constructed so that measurements could be made without impairing the sample plug hydrodynamic characteristics. The electrochemical behavior of the tubular voltammetric cell in a low-dispersion FIA manifold and the behavior of the FIA system incorporating this type of voltammetric cell intended for multisite detection were evaluated by performing measurements with potassium hexacyanoferrate(II). Feasibility of the approach was demonstrated in the sequential determination of salicylic and acetylsalicylic acids in pharmaceutical products at a fixed potential of 0.98 V. The system allows sequential determination of salicylic acid concentrations ranging from 1.0 × 10−5 to 5.0 × 10−5M and acetylsalicylic acid concentrations between 1.0 × 10−3 and 5.0 × 10−3M with good precision on both detection sites and with relative standard deviations (RSDs) ≥ 1.5% (n = 10) and 2.1% (n = 10), respectively. A comparison of these results with those of the U.S. Pharmacopeia procedure showed RSDs <5.0 and 1.0% for salicylic acid and acetylsalicylic acid, respectively. The proposed method enables 15 determinations per hour, which corresponds to the analysis of approximately 8 samples per hour. The detection limits of the methodology were approximately 3.5 × 10−6 and 1.1 × 10−5M, respectively, for the first and second monitoring sites.
Spectrophotometric Investigations of the Assay of Physiologically Active Catecholamines in Pharmaceutical Formulations
Authors: Nagaralli Basavaraj S , Seetharamappa Jaldappa , Melwanki Mahaveer B , Ramesh Kunabevu C , Keshavayya Jathi
Published: February 2020

Two simple, sensitive, and accurate spectrophotometric methods are proposed for the determination of levodopa (LD), methyldopa (MD), dopamine hydrochloride (DP), and pyrocatechol (PC) in pure and pharmaceutical preparations. The methods are based on measurement of the absorbances of tris( o-phenanthroline)iron(II) (method A) and tris(bipyridyl)iron(II) (method B) obtained by the oxidation of the catecholamines by iron(III) in the presence of 1,10-phenanthroline and 2,2′-bipyridyl at 510 and 522 nm, respectively. The absorbances were found to increase linearly with increases in the concentrations of the catecholamines, results which were corroborated by the calculated correlation coefficients (0.9990–0.9996). Beer's law was valid over the concentration ranges of 0.04–0.6, 0.06–0.75, 0.06–0.65, and 0.05–0.70 μg/mL in method A and 0.02–1.0, 0.04–1.3, 0.05–1.0, and 0.06–1.1 μg/mL in method B for PC, MD, LD, and DP, respectively. The common excipients and additives did not interfere in their determinations. The proposed methods were successfully applied to the assay of LD, MD, and DP in various dosage forms. The results were validated by statistical analysis.
Concurrent Determination of Four Fluoroquinolones in Catfish, Shrimp, and Salmon by Liquid Chromatography with Fluorescence Detection
Authors: Roybal José E , Walker Calvin C , Pfenning Allen P , Turnipseed Sherri B , Storey Joseph M , Gonzales Steve A , Hurlbut Jeffrey A
Published: February 2020

A liquid chromatographic (LC) method with fluorescence detection was developed for concurrent determination of 4 fluoroquinolones: ciprofloxacin (CIPRO), enrofloxacin (ENRO), sarafloxacin (SARA), and difloxacin (DIFLX) in catfish, shrimp, and salmon. The procedure consists of extraction from fish tissue with acidified ethanol, isolation and retention on a cation exchange solid-phase extraction column, elution with basic methanol, and LC analysis with fluorescence detection. LC is performed by isocratic elution with acetonitrile–2% acetic acid (16 + 84) mobile phase, and a PLRP-S polymer column with fluorescence detection, excitation 278 nm and emission 450 nm. A target level of 20 ppb for each of the 4 fluoroquinolones has been established for this method. Fortified and incurred fish sample results are based on a 5-point standard curve calculation (10–160 ppb). Overall percent recoveries (% relative standard deviation) from fortified catfish were 78 (10), 80 (11), 70 (9.4), and 78 (10); from fortified shrimp, 69 (5.9), 85 (4.9), 79 (5.9), and 90 (4.5); and from fortified salmon, 56 (15), 93 (5.6), 61 (11), and 87 (5.0) for CIPRO, ENRO, SARA, and DIFLX, respectively. Data from the analysis of fluoroquinolone-incurred catfish, shrimp, and salmon are presented.
Kinetic Spectrophotometric Method for the Determination of Ranitidine and Nizatidine in Pharmaceuticals
Authors: Walash Mohamed I , Belal Fathalla , Ibrahim Fawzia , Hefnawy Mohamed , Eid Manal
Published: February 2020

An accurate and simple kinetic method is described for the determination of ranitidine and nizatidine in pure form and in pharmaceuticals. The method is based on the reaction of the compounds with 7-chloro-4-nitrobenz-2-oxa-1,3-diazole in pH 7.4 borate buffer at 60°C for a fixed time of 25 min for both compounds. The absorbance of the reaction product is measured at 495 nm for ranitidine and nizatidine. Calibration graphs were linear over the concentration range of 2–20 μg/mL, with limits of detection of 0.13 (3.7 × 10−7M) and 0.25 μg/mL (7.5 × 10−7M) for ranitidine and nizatidine, respectively. The proposed method was applied successfully to the determination of ranitidine in tablets and ampoules with average recoveries of 100.26 ± 0.69 and 100.29 ± 0.59%, respectively, and to the determination of nizatidine in capsules with an average recovery of 104.26 ± 0.44%. The results obtained are in good agreement with those obtained by the other methods used for comparison. A proposal of the reaction pathway is also presented.
Detection of Salmonella in Fresh Cheese, Poultry Products, and Dried Egg Products by the ISO 6579 Salmonella Culture Procedure and the AOAC Official Method: Collaborative Study
Authors: Feldsine Philip T , Lienau Andrew H , Leung Stephanie C , Mui Linda A , Humbert Florence , Bohnert Marylène , Mooijman Kirsten , Schulten Saskia , Veld Paul In’t , Rollier Patricia , Leuschner Renata , Capps Katherine ,   Collaborators:, Agin J , Allaert C , Asmundson R , Asperger H , Bohnert M , Bound A , Dixon L , Donda S , Espersen M , Foster K , Gangar V , Hammack T , Humbert F , Humes L , in’t Veld P , James L , Jost-Keating K , Kalinowski R , Kwan J , Lamb J , Leung S , Lienau A , Littell A , Mooijman K , Mui L , Ott M , Qvist S , Roberts D , Ruby R , Rude R , Santos C , Schulten S , Sellers R , Smith M , Solis D , Stecchini M L , Stegeman H , Steneryd A , Suktankar V , Wiberg C , Young V
Published: February 2020

Three food types were analyzed for the presence of Salmonella by the AOAC culture method and by the International Organization for Standardization (ISO 6579:2002) culture method. Paired test portions of each food type were simultaneously analyzed by both methods. A total of 21 laboratories representing federal government agencies and private industry, in the United States and Europe, participated in this interlaboratory study. Foods were artificially contaminated with Salmonella and competing microflora if naturally contaminated sources were not available. No statistical differences (p < 0.05) were observed between the AOAC and ISO culture methods for fresh cheese and dried egg products. A statistically significant difference was observed for one of the 2 lots of poultry from the first trial. The poultry meat used in this run was radiation sterilized, artificially contaminated with Salmonella and competitive flora, and then lyophilized. A second trial was conducted with 2 separate lots of raw ground chicken that were naturally contaminated. The results from the second trial showed no statistical difference between the 2 culture methods. A third trial involving 4 laboratories was conducted on 2 separate lots of naturally contaminated raw poultry. Again, no statistically significant differences occurred. It is recommended that ISO 6579:2002 culture method for Salmonella be adopted Official First Action for the analysis of fresh cheese, fresh chilled and frozen poultry, and dried egg products.
Sensitivity and Specificity of the Sanita-kun Aerobic Count: Internal Validation and Independent Laboratory Study
Authors: Morita Hiroshi , Ushiyama Masashi , Aoyama Shigeyuki , Iwasaki Mihoko
Published: February 2020

The Sanita-kun Aerobic Count consists of a transparent cover film, an adhesive sheet, a layer of nonwoven fabric, and a water-soluble compound film, including a culture medium formula for detection of aerobic microorganisms. The Sanita-kun sheet was validated for 14 food categories in an internal study and an independent study was conducted on ground beef and hot dogs. Both studies showed no significant difference in performance between 5 or 8 replicates of the Sanita-kun sheets and AOAC Method 966.23, excluding some lots of foods. The correlation coefficient to plate count agar in the internal accuracy study was 0.99. The average relative standard deviation for repeatability of total foods was 0.26 and 0.19, respectively, excluding <10 average counts. The ruggedness study, which examined the influence of incubation temperature and period, recommended incubation of the Sanita-kun sheet at 32.5 ± 2.5°C for 46 ± 2 h. Comparison of 3 lots of Sanita-kun sheets showed no decrease of performance in the older lot. The shelf-life of the sheet is at least 14 months. The Sanita-kun Aerobic Counts has been granted AOAC Performance Tested MethodSM status.
Kinetic Spectrophotometric Determination of the Macrolide Antibiotic Josamycin in Formulations
Authors: Al-Majed Abdulrahman A , Belal Fathalla , Ibrahim Kamal E E , Khalil Nasr Y
Published: February 2020

A simple kinetic spectrophotometric method was developed for the determination of josamycin in its dosage forms. The method is based on oxidation of the drug with alkaline potassium permanganate at room temperature for a fixed time of 20 min and measuring the produced green color at 611 nm. The absorbance–concentration plot is rectilinear over the range of 2–10 μg/mL (2.4 × 106–1.2 × 10−5M) with minimum detectability of 1.0 μg/mL (1.2 × 10−6M). The determination of josamycin by fixed concentration and the rate-constant methods is also feasible with the calibration equations obtained, but the fixed-time method proved to be more applicable. The procedure was applied successfully to commercial tablets, and statistical analysis showed that the results compared favorably with those obtained by reference methods. The effect of sensitizers and surfactants on the performance of the proposed method was also studied. A proposal of the reaction pathway was presented.
Simultaneous Determination of Residual Antiparasitic Lactones in Bovine Muscle and Liver by Liquid Chromatography with Fluorescence Detection
Authors: Nagata Tomoko , Miyamoto Fumio , Hasegawa Yasuyuki , Ashizawa Eiichi
Published: February 2020

Abamectin, doramectin, eprinomectin, ivermectin, milbemectin, and moxidectin in bovine muscle and liver were extracted with acetonitrile. The extracts were partitioned with n-hexane and then evaporated to dryness. The residue was cleaned up on Bond Elute NH2 cartridge, and the drugs were eluted from the cartridge with methanol–ethyl acetate (3 + 7). The eluate was evaporated to dryness, and residues were derivatized with N,N-dimethyl-formamide–acetic anhyride-1-methylimidazole. The derivatives were determined by liquid chromatography with fluorescence detection. Recoveries of the 6 drugs were 79.6–63.8% in muscle and 71.6–60.6% in liver at 0.01 ppm levels. The quantitation limits were 5 ppb for each drug.
Distribution of Deoxynivalenol in Wheat, Wheat Flour, Bran, and Gluten, and Variability Associated with the Test Procedure
Authors: Samar María M , Fontán Constantino Ferro , Resnik Silvia L , Pacin Ana M , Castillo Marcelo D
Published: February 2020

Analytical data obtained on deoxynivalenol (DON) concentration in naturally contaminated wheat during processing in an industrial mill were statistically analyzed, and the distribution functions of DON concentration in lots of wheat, bran, wheat flour, and gluten were estimated. The analytical method had acceptable precision (HORRAT 0.25—0.32) for each test sample. The total variance combined sampling, sample preparation, and analytical variances were 0.188, 0.033, 0.42, and 0.0014 ppm2 for wheat, 1.93; flour, 0.99; bran, 4.68; and gluten, 0.29, respectively. The distribution function of DON contamination presented an asymmetric tail for high values of concentration in wheat grains and wheat flour; in bran it seemed to be bimodal with 2 separated peaks of different concentrations; in gluten the normal distribution function gave a reasonably good fit to empirical data. The function η(c) = –ln(–lnp), where p (c) is the cumulative distribution function was linear with c in the so-called extreme-value type I distribution and could be fitted by a cubic polynomial in c in the distributions determined for all the products. This variability and distributional information contributes to the design of better sampling plans in order to reduce the total variability and to estimate errors in the evaluation of DON concentration in lots of wheat and wheat products.
Recent Advances in the Thin-Layer Chromatography of Pesticides: A Review
Authors: Sherma Joseph
Published: February 2020

Advances in the applications of thin-layer chroma-tography (TLC) and high-performance TLC for the separation, detection, identification, and determination of pesticides, other agrochemicals, and related compounds are reviewed for the period 2000–2002. Analyses are described for a variety of samples, such as food, biological, and environmental samples, and for residues of pesticides of various types, including insecticides, herbicides, and fungicides, belonging to different chemical classes. References are included for residue analysis, hydrophobicity studies, and the use of TLC and thin-layer radiochromatography for studies of pesticide metabolism, degradation, uptake, and related topics.
Comparison of the Ammonium Oxalate Extraction of Fertilizer for K2O, Method 983.02, with the Ammonium Citrate/EDTA Extraction, Method 993.31
Authors: Newlon Natalie F
Published: February 2020

The direct available method for phosphorus in fertilizers, Method 960.03, is an Official Method for extraction of both P2O5 and K2O. Because K2O is much more soluble and easier to extract than P2O5, the conditions of the extraction procedure are set for efficient extraction of P2O5, and the extraction of K2O is, in effect, a bonus. In 1993, a modified extraction procedure, using an extractant of ammonium citrate/ethylenediaminetetraacetic acid (EDTA) solution, was evaluated for P2O5 and then collaboratively studied. This now-modified extraction procedure for phosphorus is Official Method 993.31, which is used extensively as an alternative to Method 960.03 for phosphorus because it is less labor-intensive. Method 993.31 was also evaluated in our laboratory for K2O extraction, but it was never formally collaboratively studied for K2O. To demonstrate the suitability of Method 993.31 as an extraction procedure for K2O, as well as P2O5 in fertilizers, Method 993.31 extraction for K2O was compared with Method 983.02, the traditional ammonium oxalate extraction procedure for K2O. A wide range of fertilizer samples was extracted by using both procedures. The t-test for samples containing <30% K2O had a t-value of 1.23 and a probability of 0.22, which indicates there was no significant difference in the results obtained by the 2 extraction methods. The t-test for samples containing >30% K2O had a t-value of 0.30 and a probability of 0.77, also indicating no significant difference. It is recommended that Method 983.02 be modified to include the ammonium citrate/EDTA extraction procedure as an additional option for extraction of K2O from commercial fertilizers.
Enumeration of Probiotic Pediococci in Animal Feed: Interlaboratory Study
Authors: Leuschner Renata G K , Bew Jan , Simpson Paul J , Ross Paul R , Stanton Catherine ,   Collaborators:, Adler A , Bertin G , Braconnier M , Coeuret V , Domig K , Durand H , Kneifel W , Krause M , Marmo S , Michard J , Mietke H , Olofson A S , Thalmann A , Vernoux J P , Voets A , Warmerdam C
Published: February 2020

An enumeration method to be used as official control under Council Directive 70/524/EEC for probiotic pediococci used as feed additives was validated for consideration for adoption as Comitée Européen de Normalisation (CEN) and ISO standards. Seventeen laboratories in 11 European countries carried out an interlaboratory study. A spread plate method following BS ISO 15214:1998 using 4 different agars [MRS, acidified MRS, MRS with triphenyl tetrazolium chloride (TTC), and a newly developed pediococci selective medium (PSM)] was validated. Precision data in terms of repeatability (r) and reproducibility (R) of the method for each medium using different feeding stuffs with a high and a low inoculation level were determined. Pediococci were present in the samples in mixtures with other probiotics. The enumeration of pediococci on all agars showedan RSDr value of 0.4–3.1% and an RSDR of 1.3–4.8%. MRS agar was preferred, followed by acidified MRS and MRS + TTC agar. All 4 media gave similar counts. Depending on the presence and concentration of other probiotic, such as enterococci, lactobacilli, and yeast, acidified MRS or MRS + TTC agar are recommended. The PSM was selective for pediococci and can be used if this species is present at a concentration more than 10-fold lower than other species that can grow on the MRS agars. The methodology with all 4 media is not applicable to mineral feed.
Determination of Ultratrace Bismuth in Milk Samples by Atomic Fluorescence Spectrometry
Authors: Cava-Montesinos Patricia , Cervera M Luisa , Pastor Agustín , de la Guardia Miguel
Published: February 2020

A sensitive procedure was developed for determination of bismuth (Bi) in milk samples by hydride generation atomic fluorescence spectrometry (HG–AFS) after microwave-assisted sample digestion with HNO3 and H2O2. The method provides a sensitivity of 1832 fluorescence units (ng/mL) with a detection limit of 0.01 ng/mL, which corresponds to 20 pg absolute limit of detection, equivalent to 0.50 ng/g in the original sample. Application of the methodology to cow milk samples from the Spanish market showed the presence of Bi at a concentration of 11.8–28.8 ng/g, which compared well with data obtained after dry ashing of samples and with data obtained by inductively coupled plasma–mass spectrometry after microwave-assisted digestion.
Application of Strategically Designed Sample Composition to the Rapid Analytical Screening of Milk Samples for Polychlorinated Biphenyls
Authors: Martínez Elena , Pazos Manuel , Carro Antonia M , Llompart Maria , Cela Rafael
Published: February 2020

Strategically designed sample composition (SSC) is a new technique that decreases the number of analytical determinations needed in routine screening to as few as the number of original sample specimens while providing information that is specific to them. Although this new technique has been applied to environmental studies, this paper describes its first application to food safety studies. Contamination of milk samples with polychlorinated biphenyls (PCBs) was chosen as a case study to show the usefulness and potential of the SSC technique with a fast analytical procedure that involves saponification of the samples and solid-phase microextraction of the PCBs. A total of 20 sample specimens can be analyzed in 11 determinations with excellent predictions of the positive samples and the concentration levels of the contaminants. The robustness of the strategy was investigated and demonstrated.
Determination of Fungicide Residues in White Grapes for Winemaking by Gas Chromatography with Mass Spectrometric Detection and Assessment of Matrix Effects
Authors: González Carlos Fernández , Otero Raquel Rial , Grande Beatriz Cancho , Gándara Jesús Simal
Published: February 2020

A new analytical method, based on organic solvent extraction with dichloromethane–acetone (75 + 25, v/v) followed by gas chromatography with mass spectrometric detection, is presented for the determination of residues of 10 fungicides in white grapes for vinification. Some of them (cyprodinil, fludioxonil, and pyrimethanil) have been used for only 2–3 years and, therefore, no methods are available in the scientific literature for such a screening. Quality parameters yielded good precision (relative standard deviation of <10%) and detection limits (ranging between 1 and 18 μg/kg) that are lower than the maximum residue limits (MRLs) set by the 76/895/European Economic Community (EEC) and 90/642/EEC Directives. The applicability of the method was evaluated by analysis of 5 different white grapes produced in the Rías Baixas area in Galicia (northwestern Spain) for vinification. The method showed good performance in analyses of real samples to determine whether the concentrations of the fungicides used exceeded their MRLs. The method of standard additions was found to be necessary to avoid matrix effects in the quantification of fungicide residues. Results showed that concentrations of the fungicides identified in grapes were lower than the MRLs established by the European legislation.
Validity of the Percent Reduction in Standard Deviation Outlier Test for Screening Laboratory Means from a Collaborative Study
Authors: McClure Foster D , Lee Jung-Keun , Wilson Dennis B
Published: February 2020

AOAC INTERNATIONAL recommends an outlier test that is based on the “percent reduction in standard deviation” (PRSD) for screening the highest or lowest and 2-highest or 2-lowest laboratory means from a collaborative study. The original critical values that were developed to assess the significance of the test statistics associated with the PRSD test were obtained by simulation. In this paper, we answer several questions relative to the validity of the simulated critical values and develop formulas, based on the Student's t-distribution, to compare the simulated and formula-based critical values. Assumptions and derivations of formulas are provided along with selected tabular critical values that are used to test hypotheses at various levels of significance.
Uncertainty of Analytical Determinations
Authors: de Silva Galappatti M S
Published: February 2020

Two examples of uncertainty calculation are described for determination of nitrates in solution (APHA method 4500B) and total suspended solids in water (APHA method 2540D).
High-Performance Liquid Chromatography/Mass Spectrometry Analysis of Botanical Medicines and Dietary Supplements: A Review
Authors: Sherma Joseph
Published: February 2020

This article reviews research on the qualitative and quantitative analysis by high-performance column liquid chromatography/mass spectrometry (LC/MS) and LC/tandem mass spectrometry (LC/MS/MS) of botanical drugs, drug substances or preparations, and finished botanical products. In addition, LC/MS and LC/MS/MS techniques and commercial instruments are described and compared briefly, and prospects for future use of these methods for the analysis of botanicals are suggested. Some applications of direct MS without LC are also described.
Liquid Chromatographic Determination of Pyrantel Tartrate in Medicated Formulations
Authors: Konrardy Joyce A , Burner Mary A , Garner Tommy W , Litchman Mark A , Webster Gregory K
Published: February 2020

The validation of a novel liquid chromatographic (LC) method for the determination of pyrantel tartrate in feed is presented. The method provides a significant improvement over the efficiency and precision of AOAC Official Method 978.30. The method was shown to be accurate, precise, linear, and robust for medicated articles. Unlike the official method, the LC method was shown to be a superior stability-indicating method. After the method was validated by using laboratory blends, the effectiveness of the method was demonstrated with marketed product as well.
Photostimulated Luminescence Detection of Irradiated Herbs, Spices, and Seasonings: International Interlaboratory Trial
Authors: Sanderson David C W , Carmichael Lorna A , Fisk Saffron ,   Collaborators:, Brown P , Burton Y , Clemenson S D , Hart G , Nootenboom H , Pinnioja S , Schreiber G A , Wagner; U , Wiezorek C
Published: February 2020

An interlaboratory trial was conducted to validate photostimulated luminescence (PSL) methods for herbs, spices, and seasonings. Forty products (11 herbs, 17 spices, and 12 seasonings) were purchased from a local commercial source, and randomly selected samples were irradiated with 10 kGy. Four blended products were prepared at Scottish Universities Research and Reactor Centre, mixing varying proportions of irradiated material with the untreated product. Precharacterization against a predefined threshold identified low sensitivity products (black and white peppers) and products with high natural signals (thyme, sage, parsley, and mixed herbs), both of which might be susceptible to misclassification. Precharacterization also revealed whether calibration was likely to resolve overlap between classification categories. Eight sets of screening data and 5 sets of calibrated data were returned by participants. Of the 840 samples sent, 1593 screening measurements and 788 calibrated measurements were received from 662 samples. In screening mode, participants reached definitive conclusions in 87% of cases, 99% of which were correct. Of the remaining 13%, calibration to identify low-sensitivity resolved 60% of cases. Overall, 94% of samples were correctly identified by either screening alone, or screening plus calibration; 6% remained unclassified and therefore required further investigation by thermoluminescence. The results confirm the validity of the PSL method for herbs, spices, seasonings, and blends, and emphasize the need for calibration to identify low-sensitivity samples. This method has now been adopted by the European Committee for Standardization (CEN) and the Codex Alimentarius Commission.
Liquid Chromatographic Determination of 4, 4' -Dinitrocarbanilide, the Active Component of the Infertility Agent Nicarbazin, in Chicken, Duck, Goose, and Snake Eggs
Authors: Primus Thomas M , Kohler Dennis J , Goodall Margaret A , Yoder Christi , Mathies Thomas , Miller Lowell , Johnston John J , Vercauteren Kurt
Published: February 2020

4, 4'-Dinitrocarbanilide (DNC) was extracted from chicken, duck, goose, and snake eggs and isolated by reversed-phase liquid chromatography. DNC was detected by ultraviolet absorbance at 347 nm and quantitated by comparison with a calibration standard. Recoveries of DNC from fortified control chicken, duck, goose, and snake egg samples were determined for DNC levels of 0.16, 10, and 16 μg/g. The mean recoveries from chicken, duck, goose, and snake eggs were 92 ± 4, 88 ± 9, 87 ± 7, and 95 ± 6%, respectively. The method limits of detection for DNC in chicken, duck, goose, and snake eggs ranged from 0.015 to 0.035 μg/g. The reported method is much simpler than and equally efficient as previous methods developed for the determination of DNC residues in egg contents.
Syringe-Cartridge Solid-Phase Extraction Method for Patulin in Apple Juice
Authors: Eisele Thomas A , Gibson Midori Z
Published: February 2020

A syringe-cartridge solid-phase extraction (SPE) method was developed for determination of patulin in apple juice. A 2.5 mL portion of test sample was passed through a conditioned macroporous SPE cartridge and washed with 2 mL 1% sodium bicarbonate followed by 2 mL 1% acetic acid. Patulin was eluted with 1 mL 10% ethyl acetate in ethyl ether and determined by reversed-phase liquid chromatography using a mobile phase consisting of 81% acetonitrile, 9% water, and 10% 0.05M potassium phosphate buffer, pH 2.4. Recoveries averaged 92% and the relative standard deviation was 8.0% in test samples spiked with 50 ng/mL patulin. The method appears to be applicable for monitoring apple juice samples to meet the U.S. Food and Drug Administration compliance action level of 50 μg/kg in an industrial quality assurance laboratory environment.
Estimating Deoxynivalenol in Shelled Corn Barge Lots by Measuring Deoxynivalenol in Corn Screenings
Authors: Whitaker Thomas B , Richard John L , Giesbrecht Francis G , Slate Andrew B , Ruiz Nelson
Published: February 2020

To determine if deoxynivalenol (DON) is concentrated in small corn screenings, fourteen to twenty-three 1.1 kg test samples were taken from each of 10 barges of shelled corn. Each of the 181 test samples was divided into 2 components (fines and clean) using a 5 mm screen. The clean component sample rode the 5 mm screen and the fines component sample passed through the 5 mm screen. The DON concentration in fines component sample was about 3 times the DON concentration in the clean component sample. The DON in the 181 fines and clean component samples averaged 689.0 and 206.1 ng/g, respectively. Regression equations were developed to predict the DON in the barge based upon measurements of DON in the fines component sample. The ratio of DON in the lot to DON in the fines component sample was 0.359. The coefficient of variation (CV) associated with predicting the DON concentration in a lot with 359 ng/g using a 1.1 kg test sample was 47.0%. Increasing sample size to 4.4 kg reduced the CV to 23%.