bluuebunny/crossref_metadata_2025_split huggingface dataset:
High-Throughput Analytical Techniques for Multiresidue, Multiclass Determination of 653 Pesticides and Chemical Pollutants in Tea—Part III: Evaluation of the Cleanup Efficiency of an SPE Cartridge Newly Developed for Multiresidues in Tea
Authors: Pang Guo-Fang , Fan Chun-Lin , Chang Qiao-Ying , Li Yan , Kang Jian , Wang Wen-Wen , Cao Jing , Zhao Yan-Bing , Li Nan , Li Zeng-Yin , Chen Zong-Mao , Luo Feng-Jian , Lou Zheng-Yun 
Published: August 2013

Abstract
A comparative study was conducted over three stages on the cleanup efficiency of SPE cartridge Cleanert TPT, newly developed for multigroups of pesticide residues in tea. In Stage I, different SPE cartridges C18, graphite carbon black (GCB), primary secondary amine (PSA), and amino (NH2) were purchased and combined into 12 different sequences. Through the comparative test on cleanup efficiency of 84 representative pesticides in tea, Envi-Carb GCB + PSA with a good cleanup effect was selected. In Stage II, GC/MS test results from the comparative study of the extraction efficiency of 201 pesticides spiked into green tea and Woolong tea with Cleanert TPT and Envi-Carb + PSA SPE showed that average recoveries fell within 70–110% and RSD &lt;20% for 193 and 184 pesticides, respectively, for green tea, accounting for 96.0 and 91.0% of the total number, respectively. GC/MS/MS test results also found 193 and 184 pesticides, respectively, meeting the recovery and RSD conditions, accounting for 96.0 and 91.5%, respectively, of the total number. For Woolong tea samples, GC/MS results showed that with Cleanert TPT and Envi-Carb + PSA SPE for cleanup, there were 192 and 177 pesticides, respectively, meeting the conditions, accounting for 95.5 and 88.1% of the total number, respectively. GC/MS/MS results demonstrated that there were 195 and 184 pesticides, respectively, meeting the conditions, accounting for 97.0 and 91.5% of the total number, respectively. It was seen that Cleanert TPT was superior to Envi-Carb + PSA in cleanup efficiency, whether for green or Woolong tea samples, or GC/MS or GC/MS/MS determination. In Stage III, 61 104 results of the average content value of pesticides and RSD (two teas × two Youden pair concentrations × two kinds of SPE cartridges × two instruments × 19 tests × 201 pesticides) were derived from the 19 times stability tests over 3 months by paralleling three samples every 5 days via two instruments with two kinds of SPE cartridges for cleanup, respectively, against Youden Pair samples of the 201 incurred pesticides from green and Woolong teas. The statistical analysis found that detected values from the target pesticides of the incurred Youden pair samples showed no marked differences with cleanup by either Cleanert TPT or Envi-Carb + PSA, whether for green or Woolong tea, or GC/MS or GC/MS/MS. The test results using the two aforementioned kinds of SPE cleanup for above 93% pesticides had a tolerance less than 15%, which testifies that both cartridge cleanups met the requirement for pesticide residue analysis.
Development and Validation of an Analytical Method for Quantification of Arsenic and Antimony in Liposomes Using Inductively Coupled Plasma-Optical Emission Spectrometry
Authors: Reis Priscila G , Abreu Adriana T , Guimarães Andrea G , Teixeira Mônica C , de Souza Jacqueline , Silva-Barcellos Neila M 
Published: August 2013

Abstract
Arsenic and antimony compounds are used to treat endemic diseases, such as cancer, leishmaniasis, and schistosomiasis, in spite of their toxicity. Several studies seeking the development and characterization of nanocarrier systems such as liposomes are being carried out with the aim of developing new drug delivery systems and minimizing the toxicity of these drugs. However, the lack of reference methods to quantify these semimetals within a liposomal matrix hinders the QC of these formulations. Therefore, the validation of an analytical method for arsenic and antimony quantification in liposomal matrix by inductively coupled plasma-optical emission spectrometry is presented here. The linearity, specificity, LOD, LOQ, accuracy, and precision were determined according to the International Conference on Harmonization norms and the Brazilian Health Surveillance Agency (Resolution 899). The LOD values were 0.02 and 0.06 mg/L for antimony and arsenic, respectively. The LOQ for both was 3.0 mg/L, with an adequate accuracy within 98.26 and 101.32% for different levels of antimony and 99.98 and 100.36% for arsenic. Precision (CV) was lower than 5.0%. The developed and validated method was shown to be reproducible for quantification of arsenic and antimony in liposome pharmaceutical dosage forms.
Extractive Spectrophotometric Determination of Some Nonsteroidal Anti-Inflammatory Drugs Using Methylene Blue
Authors: El-Kommos Michael E , Mohamed Niveen A , Abdel Hakiem Ahmed F 
Published: August 2013

Abstract
A simple, rapid, sensitive, and accurate extractive spectrophotometric method has been developed for the determination of seven nonsteroidal anti-inflammatory drugs (NSAIDs)—namely diclofenac sodium, ibuprofen, indomethacin, ketoprofen, ketorolac tromethamine, mefenamic acid, and naproxen—in pure forms as well as their pharmaceutical dosage forms (tablets, capsules, effervescent granules, syrups, oral drops, ampules, eye drops, gels, and suppositories). The method depends on the formation of an intensely colored ion-pair complex between the acidic drug and methylene blue in alkaline medium. The complex is stable and extractable into methylene chloride. All parameters were optimized. Beer-Lambert's law was obeyed in concentrations ranging from 0.04 to 9 μg/mL. Statistical analysis of the calibration data was carried out, and correlation coefficients were in the range from 0.9996 to 0.9998. The developed method was fully validated according to International Conference on Harmonization guidelines, and complied with U.S. Pharmacopeia guidelines. The proposed method was applied to the analysis of the investigated drugs in their pharmaceutical formulations, and good recoveries were obtained. The results obtained were compared with those of reported and official methods, and no significant differences were found with t- and F-tests. Interference effects of some compounds usually present in combination with NSAIDs were studied, and the tolerance limits of these compounds were determined.
Multivariate Optimization of Separation Conditions for Simultaneous Determination of Acemetacin and Chlorzoxazone in a Pharmaceutical Preparation by HPLC Using Response Surface Methodology
Authors: Aybaba Cigdem , Palabiyik Ismail Murat , Caglayan Mehmet Gokhan , Onur Feyyaz 
Published: August 2013

Abstract
A new, fast, accurate, precise, and sensitive RP-HPLC method for the simultaneous determination of acemetacin and chlorzoxazone has been developed. Response surface methodology with a central composite design was used to optimize the acetonitrile and ammonium acetate percentage in the mobile phase and pH of ammonium acetate. The optimum separation was achieved on a C18 column (250 × 4.6 mm id, 5 μm particle size) using the mobile phase methanol–acetonitrile–0.02 M ammonium acetate, pH 9.4 (25 + 35 + 40, v/v/v) at a flow rate of 1.5 mL/min; UV detection at 270 nm, and cyanocobalamin as an internal standard. This developed method was validated and successfully applied to a coated tablet pharmaceutical preparation.
Method Development andValidation for the Simultaneous Determination of Organochlorine and Organophosphorus Pesticides in a Complex Sediment Matrix
Authors: Alcántara-Concepción Victor , Cram Silke , Gibson Richard , de León Claudia Ponce , Mazari-Hiriart Marisa 
Published: August 2013

Abstract
The Xochimilco area in the southeastern part of Mexico City has a variety of socioeconomic activities, such as periurban agriculture, which is of great importance in the Mexico City metropolitan area. Pesticides are used extensively, some being legal, mostly chlorpyrifos and malathion, and some illegal, mostly DDT. Sediments are a common sink for pesticides in aquatic systems near agricultural areas, and Xochimilco sediments have a complex composition with high contents of organic matter and clay that are ideal adsorption sites for organochlorine (OC) and organophosphorus (OP) pesticides. Therefore, it is important to have a quick, affordable, and reliable method to determine these pesticides. Conventional methods for the determination of OC and OP pesticides are long, laborious, and costly owing to the high volume of solvents and adsorbents. The present study developed and validated a method for determining 18 OC and five OP pesticides in sediments with high organic and clay contents. In contrast with other methods described in the literature, this method allows isolation of the 23 pesticides with a 12 min microwave-assisted extraction (MAE) and one-step cleanup of pesticides. The method developed is a simpler, time-saving procedure that uses only 3.5 g of dry sediment. The use of MAE eliminates excessive handling and the possible loss of analytes. It was shown that the use of LC-Si cartridges with hexane–ethyl acetate (75 + 25, v/v) in the cleanup procedure recovered all pesticides with rates between 70 and 120%. The validation parameters demonstrated good performance of the method, with intermediate precision ranging from 7.3 to 17.0%, HorRat indexes all below 0.5, and tests of accuracy with the 23 pesticides at three concentration levels demonstrating recoveries ranging from 74 to 114% and RSDs from 3.3 to 12.7%.
Determination of Chloramphenicol Residues in Aquatic Products Using Immunoaffinity Column Cleanup and High Performance Liquid Chromatography with Ultraviolet Detection
Authors: Zhang Qing-Jie , Peng Tao , Chen Dong-Dong , Xie Jie , Wang Xiong , Wang Guo-Min , Nie Chang-Ming 
Published: August 2013

Abstract
A method based on HPLC with UV detection was developed for the quantitative determination of chloramphenicol (CAP) residues in aquatic products. The samples were extracted with ethyl acetate–ammonium hydroxide (98 + 2, v/v), followed by a cleanup step using an immunoaffinity column. The analytes were determined by HPLC-UV. Optimal conditions for the extraction and cleanup procedures are described. The linear regression equation was y = 91.47x – 8.60 with R2 = 0.9998 (y = peak area and x = CAP concentration) and showed a good reproducibility. The LOQ was 0.25 μg/kg for determining CAP spiked in the aquatic products. The mean recoveries of CAP from fish and shrimp samples fortified at 0.25–1.0 μg/kg were 88.7–93.1 and 92.0–97.3%, respectively; the repeatability RSDs were less than 8.1%. It was concluded that the method is simple, highly sensitive, and low cost for quantitatively measuring CAP residues in aquatic products. Analyte identification was confirmed by HPLC/MS/MS analysis.
Immunoaffinity Column Cleanup with LC/MS/MS for the Determination of Chloramphenicol in Honey and Prawns: Single-Laboratory Validation
Authors: Mackie Jennifer , Marley Elaine , Donnelly Carold 
Published: August 2013

Abstract
A single-laboratory validation was conducted to establish the effectiveness of an immunoaffinity column (IAC) cleanup procedure followed by LC/MS/MS for the determination of chloramphenicol (CAP) in honey and prawns. Honey is dissolved in buffer solution and centrifuged, and an aliquot applied to an IAC. For prawns, a portion of the homogenized sample is shaken with buffer and centrifuged, and an aliquot similarly applied to an IAC. For both matrix extracts, CAP is removed from the IAC with neat methanol, then directly analyzed by electrospray LC/MS/MS in the negative ionization mode using m/z 321 as a precursor ion and m/z 257 and 152 as qualifier and quantifier ions, respectively. Test portions of blank honey and prawns were fortified with CAP to give levels of 0.3, 1.0, and 5.0 μg/kg. Recoveries of CAP on 3 consecutive days ranged from 83–103% for honey and 84–108% for prawns. Based on results for fortified blank matrixes (triplicate at three levels), the RSD for repeatability (RSDr) averaged 8.4% for honey and 4.8% for prawns. The method LOD was 0.05 for prawns and 0.16 μg/kg for honey, both well below the minimum required method performance limit for CAP. The accuracy of the method was demonstrated by participation in proficiency testing, where satisfactory Z-scores were obtained for CAP in incurred samples of both honey and prawns. The method was shown to be applicable to a wide range of other matrixes, including milk, egg, royal jelly, meat, and seafood products.
Atlas™ Salmonella Detection Method Using Transcription Mediated Amplification (TMA) to Detect Salmonella enterica in a Variety of Foods and Select Surfaces
Authors: Kwong William , Livezey Kristin , Reshatoff Michael , Vaughn Steve , Freed Anna , Puente Celina , Hu Ernie , Zukowski Alexis , Schweis Franz , Yang Hua , Fleischer Chad , Kamantigue Edgar , Morgan Jarrod , Koehler Robert , Maroni Brett , Becker Michael , Wisniewski Michele 
Published: August 2013

Abstract
The Atlas™ Salmonella detection assay was compared to the reference culture methods for 12 foods and three surfaces. Comparison of the Atlas method to the U.S. Food and Drug Administration Bacteriological Analytical Manual (FDA/BAM) and U.S. Department of Agriculture-Food Safety and Inspection Service/Microbiology Laboratory Guidebook (USDA-FSIS/MLG) reference methods required an unpaired approach. Each method had a total of 320 samples inoculated with an S. enterica strain. Each food and surface was inoculated with a different strain of S. enterica at two different levels/method. Meat and egg products were compared to the USDA-FSIS/MLG 4.05 method. All other foods were compared to the FDA/BAM-5 method. The Atlas method had 148 positives out of 320 total inoculated samples, compared to 119 positives for the reference methods. Overall, the probability of detection analysis of the results showed equivalent or better performance by the Atlas Salmonella detection method compared to the reference methods. The Atlas Salmonella detection assay detected all 100 inclusive organisms and none of the 30 exclusive organisms. The lot-to-lot and kit stability studies showed no statistical differences between lots or over the term of the shelf-life. Instrument-to-instrument testing showed no statistical difference between instruments. Finally, the robustness study showed no difference when the sample volume added to the Atlas Salmonella detection assay varied by 10%, storage time was extended up to 5 days before analysis, or enrichment times were varied from 12 to 24 h.
Method for the Determination of Total Selenium in a Wide Variety of Foods Using Inductively Coupled Plasma/Mass Spectrometry
Authors: Sullivan Darryl , Zywicki Richard , Yancey Mark 
Published: August 2013

Abstract
An optimized method for use in a high volume laboratory was developed and validated for the determination of total selenium in a wide variety of food products including infant formula. The method utilizes a single-stage, closed-vessel microwave digestion procedure with nitric acid. Upon completion of digestion, the solution is brought to volume with water. A dilution is prepared for analysis by adding methanol (MeOH) to an aliquot and then brought to volume by nitric acid diluent resulting in a 3% MeOH concentration. The amount of selenium is determined by inductively coupled plasma (ICP)/MS with the capability of removing argon-based polyatomic interferences. Experiments were conducted to validate the method by determining precision, accuracy, linearity, specificity, ruggedness, and robustness. The calculated practical reporting level for this method was 25.0 μg/kg. The method provided an average RSD of 2.03% during analysis of a wheat flour reference material and 2.73% during analysis of a powdered infant formula. The accuracy of the method for these materials was 98.6 and 105%, respectively. The method has also been used successfully on a variety of foods from various categories including fruits, grains, vegetables, protein, and dairy.
Determination and Confirmation of Narasin and Monensin in Chicken, Swine, and Bovine Tissues by LC/MS/MS: Final Action 2011.24
Authors: Lombardi Kimberly R , Burnett Thomas J , Brunelle Sharon L , Ulrey W Dennis , Coleman Mark R ,   Collaborators:, Boison J , Connolly P , Danaher M , D’Angelo D , MacDougall J , Matus J , Rodewald J M , Ruiz S , Spilsbury L , Stephenson C , Song H , Zuidema T 
Published: August 2013

Abstract
A multilaboratory study was conducted to validate the reproducibility of AOAC Official MethodSM 2011.24 for determination of narasin and monensin in chicken, swine, and bovine tissues. This study was intended to satisfy requirements for Final Action status through the AOAC Expert Review Panel process. Ten laboratories participated in the study, analyzing blind duplicates of five incurred residue materials for each analyte. After removal of invalid data sets, the method reproducibility (RSDR 12.8–60.6%, HorRat 0.45–1.47) was within AOAC acceptance criteria. The method was awarded Final Action status by the Official Methods Board on October 4, 2012.
Determination and Confirmation of Parent and Total Ractopamine in Bovine, Swine, and Turkey Tissues by Liquid Chromatography with Tandem Mass Spectrometry: Final Action 2011.23
Authors: Ulrey W Dennis , Burnett Thomas J , Brunelle Sharon L , Lombardi Kimberly R , Coleman Mark R 
Published: August 2013

Abstract
A multilaboratory study of AOAC Official MethodSM 2011.23 was performed to satisfy requirements for Final Action status through the AOAC expert review panel process. The study included nine collaborating laboratories from the United States, Canada, Brazil, and The Netherlands. Five incurred residue materials (bovine muscle, bovine liver, swine muscle, swine liver, and turkey muscle) were analyzed by each laboratory as blind duplicates for parent and total ractopamine content. After removal of invalid data, the parent and total ractopamine methods demonstrated acceptable reproducibility (RSDR 11.4–42.4%, HorRatR 0.34–2.01) based on AOAC criteria. The method was awarded Final Action status by the Official Methods Board on October 4, 2012.
Flavanol and Procyanidin Content (by Degree of Polymerization 1–10) of Chocolate, Cocoa Liquors, Cocoa Powders, and Cocoa Extracts: First Action 2012.24
Authors: Robbins Rebecca J , Leonczak Jadwiga , Li Julia , Johnson J Christopher , Collins Tom , Kwik-Uribe Catherine , Schmitz Harold H ,   Collaborators:, Austad J , Bhandari S , Cifuentes T , Derck V , Ellem S , Ellingson D , Gallegos T , Groves M , Grypa R , Gu L , Hongyu W , Huang D , Johnson J C , Jones M , Kremers B , Kuhnle G , Li J , Mateos A R , Ottaviani J , Schaneberg B , Spencer J , Sullivan D , Vidts K , Wang W , Williamson G , Zapf M 
Published: August 2013

Abstract
An international collaborative study was conducted on an HPLC method with fluorescent detection for the determination of flavanols and procyanidins in chocolate and cocoa-containing materials. The sum of the oligomeric fractions with degree of polymerization 1–10 was the determined content value. Sample materials included dark and milk chocolates, cocoa powder, cocoa liquors, and cocoa extracts. The content ranged from approximately 2 to 500 mg/g (defatted basis). Thirteen laboratories—representing commercial, industrial, and academic institutions in six countries—participated in this interlaboratory study. Fourteen samples were sent as blind duplicates to the collaborators. Results for 12 laboratories yielded repeatability RSD (RSDr) values below 10% for all materials analyzed, ranging from 4.17 to 9.61%. Reproducibility RSD (RSDR) values ranged from 5.03 to 12.9% for samples containing 8.07 to 484.7 mg/g material analyzed. In one sample containing a low content of flavanols and procyanidins (approximately 2 mg/g), the RSDR was 17.68%.
ComparativeValidation Study To Demonstrate the Equivalence of a Minor Modification to AOAC Official Method 2005.04 Assurance GDS® E. coli O157:H7 Method to the Reference Culture Method: 375 Gram Sample Size
Authors: Feldsine Philip T , Montgomery-Fullerton Megan , Roa Nerie , Kaur Mandeep , Lienau Andrew H , Jucker Markus , Kerr David E 
Published: August 2013

Abstract
The Assurance GDS® Escherichia coli (E. coli) O157:H7, AOAC Official MethodSM 2005.04, has been modified to include a larger sample size of 375 g. A methods comparison study was conducted to demonstrate the equivalence of this modification to the reference culture method. Ninety samples and controls, representing three foods, were analyzed. Results show no statistically detectable difference between the Assurance GDS E. coli O157:H7 assay and the reference culture methods for the detection of E. coli O157:H7, other than the low level of inoculation for leaf lettuce, for which the GDS gave noticeably higher recovery [difference in probability of detection between candidate methods (dPODc = +0.45)]. There were also suggestions of moderate differences (dPODc = +0.15 to +0.20) for ground beef and the high level of leaf lettuce, but the study size was too small to detect differences of this size. Results showed that the Assurance GDS E. coli O157:H7 method is equivalent to reference culture methods for the detection of E. coli O157:H7.
Comparative Validation Study to Demonstrate the Equivalence of a Minor Modification to AOAC Official Method 2005.05 Assurance GDS® Shiga Toxin Genes (O157) Method to the Reference Culture Method: 375 Gram Sample Size
Authors: Feldsine Philip T , Montgomery-Fullerton Megan , Roa Nerie , Kaur Mandeep , Kerr David E , Lienau Andrew H , Jucker Markus 
Published: August 2013

Abstract
The Assurance GDS® Shiga Toxin Genes (O157), AOAC Official MethodSM 2005.05, has been modified to include a larger sample size of 375 g. A methods comparison study was conducted to demonstrate the equivalence of this modification to the reference culture method. Ninety samples and controls, representing three foods, were analyzed. Results show no statistically detectable difference between the Assurance GDS Escherichia coli O157:H7 assay and the reference culture methods for the detection of E. coli O157:H7, other than the low level of inoculation for leaf lettuce for which the GDS gave noticeably higher recovery [difference in Probability of Detection between candidate methods (dPODc = +0.45)]. There were also suggestions of moderate differences (dPODc = +0.15 to +0.20) for ground beef and the high level of leaf lettuce, but the study size was too small to detect differences of this size. Results showed that the Assurance GDS Shiga Toxin Genes (O157) method is equivalent to the reference culture methods for the detection of Shiga toxigenic E. coli O157:H7.