bluuebunny/crossref_metadata_2025_split huggingface dataset:
Analytical Utility of Quadrupole Time-of-Flight Mass Spectrometry for the Determination of Pesticide Residues in Comparison with an Optimized Column High-Performance Liquid Chromatography/Tandem Mass Spectrometry Method
Authors: Picó Yolanda , Blasco Cristina , Farré Marinella , Barceló Damiá 
Published: February 2020

Abstract
A multiresidue method for the analysis of 30 pesticides with different physicochemical properties in fruits and vegetables was developed. The method involves a rapid and small-scale extraction procedure based on matrix solid-phase dispersion using octadecylsilyl (C18) as the dispersant and dichloromethane as the eluent. The target pesticides were determined using column high-performance liquid chromatography/triple quadrupole-tandem mass spectrometry (LC/QqQ-MS/MS). The method was validated for sensitivity, linearity, reproducibility, and accuracy. A recovery study was conducted at 3 different levels, and the average ranged from 74 to 99 for all of the studied compounds, with relative standard deviations lower than 19. The proposed method achieved limits of quantitation between 0.5 and 10 g/kg, well below the maximum residue limits. The capability of the extraction procedure to extract pesticide residues other than those selected as target analytes has been checked by ultra-performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UPLC/QqTOF-MS). Four incurred pesticides, not covered in the method as target analytes, were identified and unequivocally confirmed. Both systems were demonstrated to be complementary. LC/QqQ-MS/MS has the advantage that its detection limits are somewhat lower, and UPLC/QqTOF-MS offers the possibility to identify pesticides and transformation products not included as targets of the study.
Detection of the Potential Adulterant Teucrium chamaedrys in Scutellaria baicalensis Raw Material and Extract by High-Performance Thin-Layer Chromatography
Authors: Hong Thao , Jeong Mijeong Lee , Zahn Michael , Fay Brooke A , Lee Kangwoo , Hwangbo Huunjung , Park Eunhye , Kim Minjung , Ma Wenwen 
Published: February 2020

Abstract
Teucrium chamaedrys (Gemander) has been reported as an adulterant of Scutellaria lateriflora (American skullcap) herbal preparations and is also known to be hepatotoxic. A quick and simple high-performance thin-layer chromatographic (HPTLC) method was developed for the detection of T. chamaedrys (Germander) in S. baicalensis (Chinese skullcap) extract, an ingredient of the proprietary blend product, Univestin. The HPTLC profile of T. chamaedrys was distinguished from that of S. baicalensis by its bright green fluorescence bands. This simple method can be completed in an hour for the quality control of Univestin and its raw material, S. baicalensis. The method is sensitive and can detect T. chamaedrys at levels as low as 0.5 (w/w).
Determination of the Anti-Osteoporosis Drug Ipriflavone in Pharmaceutical Formulation by Stripping Voltammetric and Chromatographic Methods
Authors: El-Desoky Hanaa S , Beltagi Amr M , Ghoneim Mohamed M 
Published: February 2020

Abstract
Ipriflavone is a nonhormonal isoflavone derivative currently used as a bone-building agent for prevention and treatment of postmenopausal osteoporosis. Ipriflavone was reduced at the hanging mercury drop electrode in buffers of pH 211 via the consumption of 2 electrons corresponding to the reduction of the C=O double bond in the C 4 position of the analyte molecule. A fully validated square-wave adsorptive cathodic stripping (SW-AdCS) voltammetric method was described for the trace quantification of bulk ipriflavone. A linear response, with concentrations of bulk ipriflavone over the range 5 1094 107 M with a limit of detection of 1.5 109 M bulk ipriflavone, was obtained. Moreover, an LC-UV detection method was also described for determining ipriflavone. The peak area was proportional to the concentration of bulk ipriflavone over the range 1 1071 104 M with a limit of detection of 3 108 M. The described SW-AdCS voltammetric and LC methods were successfully applied for the assay of ipriflavone in iprivone&lt;sup/&gt; tablets without interference from excipients. Accuracy and precision of both methods for determination of ipriflavone in its tablets were studied and discussed.
Optimization of the Treatment of Wheat Samples for the Determination of Phytic Acid by HPLC with Refractive Index Detection
Authors: Amaro Rosa , Murillo Miguel , Gonzlez Zurima , Escalona András , Hernández Lus 
Published: February 2020

Abstract
The treatment of wheat samples was optimized before the determination of phytic acid by high-performance liquid chromatography with refractive index detection. Drying by lyophilization and oven drying were studied; drying by lyophilization gave better results, confirming that this step is critical in preventing significant loss of analyte. In the extraction step, washing of the residue and collection of this water before retention of the phytates in the NH2 Sep-Pak cartridge were important. The retention of phytates in the NH2 Sep-Pak cartridge and elimination of the HCl did not produce significant loss (P = 0.05) in the phytic acid content of the sample. Recoveries of phytic acid averaged 91, which is a substantial improvement with respect to values reported by others using this methodology.
Determination of Bromoxynil Octanoate in Soil and Corn by GC with Electron Capture and Mass Spectrometry Detection Under Field Conditions
Authors: Liu Xin-Gang , Dong Feng-Shou , Zheng Yong-Quan , Li Yuan-Bo 
Published: February 2020

Abstract
In this paper, a simple, and rapid analysis of bromoxynil octanoate is reported for soil, corn leaves, and corn seeds by utilizing one-step liquid-liquid extraction and partitioning, followed by GC with electron capture (ECD) and mass spectrometry (MS) detection. The method was validated by recovery experiments and assessment of matrix effects. Recoveries for GC-ECD and GC/MS were 82.3110.7 with a relative standard deviation of &lt;14 using matrix-matched calibration solutions for quantification. The limit of quantitation (LOQ) values were 0.005 and 0.2 mg/kg for the ECD and MS detector, respectively, depending on the sensitivity of the target compound. The concentration levels for bromoxynil octanoate residue found in soil, corn leaves, and corn seeds from field experiments were clearly below the LOQ of the ECD detector. The half-life times of bromoxynil octanoate were 2.24.2 days in soil and corn leaves. These results indicated that the developed method was appropriate for analysis of bromoxynil octanoate in soil and corn samples.
LC Determination of Albiflorin and Paeoniflorin in Bai Shao (Paeonia lactiflora) as a Raw Herb and Dried Aqueous Extract
Authors: Lee Samiuela , Khoo Cheang S , Hennell James R , Pearson Jarryd L , Jarouche Mariam , Halstead Clynton W , Bensoussan Alan 
Published: February 2020

Abstract
A validated analytical method is reported for the analysis of paeoniflorin and albiflorin in Bai Shao (Paeonia lactiflora) as a dried raw herb and commercially prepared dried aqueous extract. The samples were extracted by sonication in methanol and the extract analyzed by LC-photodiode array with identity confirmation by electrospray ionization-tandem MS. A C18 column was used with an acetonitrilewater gradient mobile phase. Paeoniflorin and albiflorin were quantified at 230 nm. Ions with m/z 121 and 327 were produced with the MS detector, using the paeoniflorin precursor ion with m/z 479. For albiflorin, the precursor ion with m/z 479 produced the m/z 121 and 77 ions. The amounts of paeoniflorin and albiflorin found in the raw herb were 33.2 and 1.8 mg/g, respectively; and in the dried aqueous extract, the amounts were 34.8 and 15.7 mg/g, respectively. The LODs for paeoniflorin and albiflorin were 0.37 and 1.39 mg/g, respectively, for the raw herb and 0.25 and 0.06 mg/g, respectively, for the dried aqueous extract.
Simultaneous Identification and Quantitative Determination of Selected Aminoglycoside Antibiotics by Thin-Layer Chromatography and Densitometry
Authors: Hubicka Urszula , Krzek Jan , Woltyska Hanna , Stachacz Boóena 
Published: February 2020

Abstract
A TLCdensitometric method has been developed for simultaneous identification and quantitative determination of amikacin, gentamicin, kanamycin, neomycin, netilmicin, and tobramycin. This separation of antibiotics was achieved on silica gel TLC plates without a fluorescent indicator and with methanol25 ammoniachloroform (3 + 2 + 1, v/v/v) as the mobile phase. The densitometric measurements were made at 500 nm after detection with a 0.2 ninhydrin solution in ethanol. Under these conditions, good separation of the chosen aminoglycosides was obtained. The method is distinguished by high sensitivity, with the LOD from 0.25 g for amikacin to 1.00 g for gentamicin and the LOQ from 0.5 g for amikacin to 1.65 g for gentamicin, and a wide linearity range 0.756.25 g/spot for amikacin and netilmicin and 1.512.50 g/spot for other antibiotics. The precision of the determination was very good; RSD varied in the range 0.30.6.
Levels of Trans Fats in Diets Consumed in Developing Economies
Authors: Butt Masood Sadiq , Sultan Muhammad Tauseef 
Published: February 2020

Abstract
Cardiovascular complications are a leading cause of mortality worldwide, and dietary patterns and lifestyle are key factors responsible for their progression. Sedentary lifestyle and transient changes in nutrition have led to drastic increases in such maladies during the last few decades, and dietary changes are significant, as they are coupled with high fat intake, especially Trans fats. In developed countries, legislations and monitoring systems have resulted in reduced consumption of these metabolites. The developing world, especially South Asia, is also facing the menace of Trans fats; lack of governmental interest and ignorance among consumers are the main reasons. In these regions, the use of hydrogenated vegetable oil (ghee) and shortening in deep-fat frying of culinary items, such as samosa, paratha, bhatura, poori, and tikkies, results in increased consumption of Trans fats. Research investigations and cohort studies showed a positive correlation between consumption of Trans fats and cardiovascular disorders. In this article, Trans fats intake and its level in different products available in developing countries, particularly in South Asia, were reviewed along with information regarding processes involved in the production and possible reduction of Trans fats.
Spectrofluorometry, Thin Layer Chromatography, and Column High-Performance Liquid Chromatography Determination of Rabeprazole Sodium in the Presence of Its Acidic and Oxidized Degradation Products
Authors: Osman Afaf , Osman Mohamed 
Published: February 2020

Abstract
The objective of this study is to develop validated stability-indicating spectrofluorometric, TLC-densitometric, and HPLC methods for the determination of rabeprazole sodium and its degradation products. The first method was based on measuring the fluorescence intensity of the drug at 416 and 311 nm for the emission and at 320 and 274 nm for the excitation for acid and oxidized solutions, respectively. The second method was based on the separation of the drug from its acidic and oxidized degradation products followed by densitometric measurement of the intact drug spot at 284 nm. The separation was carried out on Fluka TLC sheets of silica gel 60 F254 using isopropyl alcohol30 ammonia (80 + 2, v/v) mobile phase. The third method was based on HPLC separation of rabeprazole sodium from its acidic and oxidized degradation products on a reversed-phase Waters Nova-Pak C18 column using 0.05 M potassium dihydrogen phosphatemethanolacetonitrile (5 + 3 + 2, v/v/v) pH 7 0.2 mobile phase. The proposed procedures were successfully applied for the determination of rabeprazole sodium in pure form, laboratory-prepared mixtures, tablet, and expired batch. The obtained results were statistically compared with those of a reported method and validated according to United States Pharmacopeia guidelines. Two main acidic degradation products of the drug were separated and subjected to IR spectrometry and MS to confirm their structures, and the schemes for their formation were elucidated.
Validation of the Soleris® Yeast and Mold Test for Semiquantitative Determination of Yeast and Mold in Selected Foods
Authors: Alles Susan , Shrestha Nabina , Ellsworth Amanda , Rider Alicia , Foti Debra , Knickerbocker Jake , Mozola Mark 
Published: February 2020

Abstract
The Soleris yeast and mold method, a growth-based test system with an optical detection end point, was evaluated for its ability to detect yeast and mold contamination in a wide variety of foods. The Soleris test was used in a semiquantitative manner, in which the test result is positive or negative at a threshold level determined by the dilution and volume of sample homogenate added to the Soleris test vial. By testing at two or more threshold levels, the contamination level can be estimated. The LOD of the Soleris method is 10 CFU/g when 1 mL of a 1:10 sample homogenate is added to the test vial. In these studies, the Soleris results were compared to plate counts obtained using the U.S Food and Drug Administration/Bacteriological Analytical Manual direct plating method, and agreement between the methods was calculated.Considering results from both internal and independent laboratory trials, overall agreement between the methods was 90. Chi-square analysis showed, with few exceptions, that results of the Soleris and direct plating methods were not statistically different. Ruggedness testing was performed, and the Soleris method was found to be robust when challenged with marginally suboptimal assay conditions. Results of inclusivity testing showed that the Soleris test vial medium supports the growth of a wide variety of yeasts and molds common to foods. Results of exclusivity testing showed that bacteria do not produce positive results, even when present in the vial in relatively high initial concentrations. The Solerismethod produces results in 72 h or less and thus offers considerable time savings in comparison to other commonly used yeast and mold methods.
Reversed-Phase Liquid Chromatographic Determination of Two Manufacturing Intermediates in D&C Red No. 34 and Its Lakes
Authors: Harp Bhakti Petigara , Barrows Julie N 
Published: February 2020

Abstract
A reversed-phase LC method was developed to determine two manufacturing intermediates in the monosulfo monoazo color additive D&C Red No. 34 and its lakes. The analytes are 2-amino-1-naphthalenesulfonic acid (Tobias acid) and 3-hydroxy-2-naphthalenecarboxylic acid (3-hydroxy-2-naphthoic acid). This method can be used for batch certification of the color additives by the U.S. Food and Drug Administration to ensure that each lot meets published specifications for coloring drugs and cosmetics. The new method uses lithium oxalate in methanolwater to dissolve the color additives for analysis. The analytes were identified by comparison of their LC retention times and UV absorption spectra with those of standards. Peak area calibrations were generally linear (R &gt; 0.999) and recoveries were 105 for Tobias acid and 103 for 3-hydroxy-2-naphthoic acid. The limits of determination (LOD) were 0.01 for Tobias acid and 0.03 for 3-hydroxy-2-naphthoic acid. The RSDs at the specification levels were 0.9 for Tobias acid and 3.2 for 3-hydroxy-2-naphthoic acid. Survey analyses of 14 samples of certified D&C Red No. 34 straight colors and lakes from six domestic and foreign manufacturers yielded results for Tobias acid that generally agreed with results previously obtained by using a gravity elution column chromatographic method. Nine of the results for 3-hydroxy-2-naphthoic acid were 2 to 5 times higher than the results obtained using the column chromatographic method. We attribute the lower accuracy of the column chromatographic method to incomplete solubility of the samples using the method conditions and difficulty with interpreting the UV spectrophotometric results.
A Square-Wave Adsorptive Stripping Voltammetric Method for Determination of Fast Green Dye
Authors: Al-Ghamdi Ali F 
Published: February 2020

Abstract
Square-wave adsorptive stripping voltammetric (SW-AdSV) determinations of trace concentrations of the coloring agent fast green were described. The analytical methodology used was based on the adsorptive preconcentration of the dye on the hanging mercury drop electrode, and then a negative sweep was initiated. In pH 10 carbonate supporting electrolyte, fast green gave a well-defined and sensitive SW-AdSV peak at 1220 mV. The electroanalytical determination of this dye was found to be optimized in carbonate buffer (pH 10) with the following experimental conditions: accumulation time (120 s); accumulation potential (0.8 V); scan rate (800 mV/s); pulse amplitude (90 mV); frequency (90 Hz); surface area of the working electrode (0.6 mm2); and the convection rate (2000 rpm). Under these optimized conditions, the AdSV peak current was proportional over the concentration range 2 1086 107 M (r = 0.999), with an LOD of 1.63 1010 M (0.132 ppb). This analytical approach possessed more enhanced sensitivity than conventional chromatography or spectrophotometry, and was simple and quick. The precision of the method in terms of RSD was 0.17, whereas the accuracy was evaluated via the mean recovery of 99.6. Possible interferences by several substances usually present as food additive azo dyes (E110, E102, E123, and E129), natural and artificial sweeteners, and antioxidants were also investigated. Applicability of the developed electroanalysis method was illustrated via the determination of fast green in ice cream and soft drink samples.
Comparison of Signal-to-Noise, Blank Determination, and Linear Regression Methods for the Estimation of Detection and Quantification Limits for Volatile Organic Compounds by Gas Chromatography
Authors: Sanagi M Marsin , Ling Susie L , Nasir Zalilah , Hermawan Dadan , Wan Ibrahim Wan Aini , Naim Ahmedy Abu 
Published: February 2020

Abstract
LOD and LOQ are two important performance characteristics in method validation. This work compares three methods based on the International Conference on Harmonization and EURACHEM guidelines, namely, signal-to-noise, blank determination, and linear regression, to estimate the LOD and LOQ for volatile organic compounds (VOCs) by experimental methodology using GC. Five VOCs, toluene, ethylbenzene, isopropylbenzene, n-propylbenzene, and styrene, were chosen for the experimental study. The results indicated that the estimated LODs and LOQs were not equivalent and could vary by a factor of 5 to 6 for the different methods. It is, therefore, essential to have a clearly described procedure for estimating the LOD and LOQ during method validation to allow interlaboratory comparisons.
1-2 Test
Authors: Feldsine Philip , Hammack Thomas 
Published: February 2020

Abstract
A study was conducted to determine the efficacy of detecting low contamination levels of Salmonella in peanut butter using the 1-2 Test. This study was conducted under the AOAC Research Institute Emergency Response Validation program. A set of samples was analyzed by the 1-2 Test and the U.S. Food and Drug Administration's Bacteriological Analytical Manual reference method. Among the 90 total samples and controls, 32 samples were positive by the 1-2 Test and the reference method. Statistical analyses of these paired samples indicated that for all levels analyzed, the difference between the 1-2 Test and reference method results were not statistically different at the 5 level.
TRANSIA PLATE Salmonella Gold
Authors: Feldsine Philip , Hammack Thomas 
Published: February 2020

Abstract
A study was conducted to determine the efficacy of detecting low contamination levels of Salmonella in peanut butter using TRANSIA PLATE Salmonella Gold (TPSG). This study was conducted under the AOAC Emergency Response Validation program. A set of samples was each analyzed by the TPSG method and the U.S. Food and Drug Administration's Bacteriological Analytical Manual reference method. Among the 45 total samples and controls, 26 were positive by the TPSG and 24 were positive by the reference method. Statistical analyses of these unpaired samples indicated that for all levels analyzed, the difference between the TPSG and reference method results were not statistically different at the 5 level.
VIDAS Salmonella (SLM) Assay Method EasySLM with ChromID Salmonella (SM2) Agar
Authors: Johnson Ronald , Mills John , Coln-Reveles Judith , Hammack Thomas 
Published: February 2020

Abstract
A method modification study was conducted for the VIDAS Salmonella (SLM) assay (AOAC Performance Tested MethodSM 020901) using the EasySLM method to validate a matrix extension for peanut butter. The VIDAS EasySLM method is a simple enrichment procedure compared to traditional Salmonella methods, requiring only pre-enrichment and a single selective enrichment media, Salmonella Xpress 2 (SX2) broth. SX2 replaces the two selective broths in traditional methods and eliminates the M broth transfer, incubation, and subsequent pooling of M broths prior to VIDAS assay. The validation study was conducted under the AOAC Research Institute Emergency Response Validation program. VIDAS SLM was compared to the U.S. Food and Drug Administration's Bacteriological Analytical Manual (FDA-BAM) method for detection of S. enterica ser. Typhimurium in peanut butter. All peanut butter samples were prepared, blind-coded, and shipped to the method developers' laboratory by Q Laboratories. In addition, Q Laboratories performed most probable number and reference method analyses on peanut butter samples. The VIDAS EasySLM ChromID Salmonella (SM2) Agar was previously validated in the Performance Tested Methods program for the detection of Salmonella in roast beef, raw ground pork, turkey, pork sausage, raw chicken breast, dry pet food, whole milk, ice cream, bagged spinach, shrimp (raw, peeled), raw cod, spent irrigation water, pecans, peanut butter, dry pasta, cake mix, ground black pepper, nonfat dry milk, liquid eggs, cantaloupe, and orange juice. In the matrix extension study for peanut butter, the VIDAS EasySLM method was shown to be equivalent to the appropriate reference culture procedure using both buffered peptone water pre-enrichment and the FDA-BAM lactose pre-enrichment in the two-step enrichment method with SX2 media. The current study extends the validation to include peanut butter.
Recognition of Gliadin and Glutenin Fractions in Four Commercial Gluten Assays
Authors: Allred Laura K , Ritter Bruce W 
Published: February 2020

Abstract
Gluten sensitivity affects nearly 1 of the population in the United States and Europe. To help these consumers avoid the health issues that result from gluten consumption, the U.S. Food and Drug Administration is attempting to establish a definition and testing protocol for gluten-free foods. Establishing this protocol depends on accurate tests that can detect and quantitate gluten. There are multiple immunoassays available for the quantitation of gluten, and most are based on one of two antibodies. These antibodies, known as the Skerritt and R5 antibodies, were examined through the use of four commercial test kits for their ability to detect the two main components of gluten, known as gliadin and glutenin, in wheat. Commercial tests based on the Skerritt and R5 antibodies demonstrated differing affinities for gliadin and glutenin, with the Skerritt-based tests recognizing glutenins more strongly, and the R5 tests recognizing gliadins more strongly. Analysis of 40 processed food samples of unknown gluten content revealed differences in gluten detection and quantitation between the Skerritt-based and R5-based assays. These discrepancies in test results may be the result of the antibody affinity differences between the Skerritt- and R5-based tests, the solubility differences between gliadins and glutenins, or a combination of these and other factors.