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Journal of AOAC International

Ramzia I El-Bagary, Ehab F Elkady, Shereen Mowaka, Maria A Attallah
A simple, accurate, and precise LC method with a reversed stationary phase was developed and validated for the determination of perindopril (PER) arginine, amlodipine (AML), and indapamide (IND) alone and in binary mixtures (PER arginine is found in two dosage forms, i.e., with either AML or IND). Chromatographic separation was carried out on a BDS Hypersil<sup>®</sup> C18 column (100 × 3 mm, 5 μm). The mobile phase, consisting of 0.05 M potassium dihydrogen phosphate buffer (pH 2.6)-methanol(50 + 50, v/v), was pumped through the column whose temperature was maintained at 50°C at a flow rate of 0...
February 7, 2017: Journal of AOAC International
Emad R Attallah, Mostafa Soliman, Mohamed M Abo-Aly
A simple, modified quick, easy, cheap, effective, rugged, and safe procedure was developed for the determination of diquat in potato using reversed-phase LC coupled with tandem MS (MS/MS) in a total run time of 10 min. Different sample preparation parameters (pH modifier type, sample size, and elevated temperature) were tested and optimized. Potato sample was extracted with acetonitrile in the presence of ammonium hydroxide at 80°C. Phase separation was obtained by shaking the extract with magnesium sulfate and sodium chloride, and analysis was done using LC-MS/MS...
February 2, 2017: Journal of AOAC International
Liang Zou, Lili Sun, Hui Zhang, Wenkai Hui, Qiaogen Zou, Zheying Zhu
The characterization of process-related impurities and degradation products of safinamide mesilate (SAFM) in bulk drugand a stability-indicating HPLC method for the separation and quantification of all the impurities were investigated. Four process-related impurities (Imp-B, Imp-C, Imp-D, and Imp-E) were found in the SAFM bulk drug. Five degradation products (Imp-A, Imp-C, Imp-D, Imp-E, and Imp-F) were observed in SAFM under oxidative conditions. Imp-C, Imp-D, and Imp-E were also degradation products and process-related impurities...
February 2, 2017: Journal of AOAC International
Jamshed Ali, Mustafa Tuzen, Tasneem G Kazi
Supramolecular solvent–based dispersive liquid–liquid microextraction was used as a preconcentration method for the determination of trace levels of Hg. This simple method accurately measured oxidized Hg<sup>II</sup> content in claystone and sandstone samples obtained from the Thar Coalfield in Pakistan. Cold vapor atomic absorption spectrometry was used as the detection technique because it is reliable and accurate. The Hg<sup>II</sup> in acidic media forms a complex with dithizone (DTz) in the presence of supramolecular solvent (tetrahydrofuran and 1-undecanol), forming reverse micelles...
February 1, 2017: Journal of AOAC International
Joe O Boison, Patricia Dowling, Johanna L Matus, Jana Kinar, Ron Johnson
This study reports the use of two validated LC with tandem MS (MS/MS) methods to study the residue depletion profile ofphenylbutazone (PBZ) and its metabolite oxyphenbutazone (OXPBZ) from equine serum, urine, and muscle, kidney, and liver tissues. One LC-MS/MS method, with an LOQ of 1.0 ng/mL for PBZ and 2.0 ng/mL for OXPBZ, was used for the analysis of the two drugs in the biological fluids (equine urine and serum); the other LC-MS/MS method, with an LOQ of 0.5 ng/g for PBZ and OXPBZ, was used for the analysis of the drugs in the equine tissue samples...
February 1, 2017: Journal of AOAC International
Gagan Jyot, Balwinder Singh
An easy and simple analytical method was standardized and validated for the estimation of residues of thiamethoxam andits metabolites in cotton. The samples were extracted with acetonitrile, water, and methanol; diluted with brine solution; partitioned into dichloromethane and ethyl acetate; dried over anhydrous sodium sulfate; and cleaned up by glass column chromatography. Final clear extracts were concentrated under vacuum and reconstituted into HPLC grade acetonitrile, and residues were estimated using an HPLC instrument equipped with a C<sub>18</sub> column and photodiode array detector system...
January 28, 2017: Journal of AOAC International
Qing-An Zhang, Xiao-Li Zhang, Yan-Ying Yan, Xue-Hui Fan
In this paper, the antioxidant capacities and compositions of two commercialized tea products and extracts from Fuzhuanbrick tea (FBT) were investigated using three HPLC methods comparing the retention times of injected standards. Principal component analysis and DPPH-spiking HPLC analysis were used to analyze correlation between antioxidant capacity and the compounds detected to screen which compounds contribute to antioxidant activity. Results indicated that all samples contained high amounts of polysaccharides, phenols, and flavonoids and had good antioxidant activity and a high level of correlation among them...
January 21, 2017: Journal of AOAC International
Grazielle Prado Alexandre, Márcio Nardelli Wandermuren, Adriano Peron, Vanessa Franco Tavares, Denis Alexandre Ramalho Padeiro, Kelly Alessandra Sakiara, María Segunda Aurora-Prado, Anil Kumar Singh, Erika Rosa Maria Kedor-Hackmann, Maria Inês Rocha Miritello Santoro
Nadolol is a blocking agent with activity in β-adrenergic receptors. The objective of this research was to develop andvalidate an HPLC and circular dichroism method for the quantification of four nadolol stereoisomers in capsules. The HPLC method was validated using a Chiralcel OD column (250 × 4,6 mm, 10 μm). The mobile phase consisted of hexane-ethanol-diethylamine-acetic acid(86 + 14 + 0.3 + 0.3, v/v/v/v), with a flow rate of 0.7 mL/min and temperature of 25 ± 1°C and UV detection carried out at 220 nm...
January 21, 2017: Journal of AOAC International
Bassam M Ayoub
Introducing green analysis to pharmaceuticalproducts is considered a significant approach topreserving the environment. This method can be anenvironmentally friendly alternative to the existingmethods, accompanied by a validated automatedprocedure for the analysis of a drug with the lowestpossible number of samples. Different simplespectrophotometric methods were developed forthe simultaneous determination of empagliflozin(EG) and metformin (MT) by manipulating their ratiospectra in their application on a recently approvedpharmaceutical combination, Synjardy tablets...
January 20, 2017: Journal of AOAC International
Amira F El-Yazbi
Sofosbuvir (SOFO) was approved by the U.S. Food and Drug Administration in 2013 for the treatment of hepatitis C virusinfection with enhanced antiviral potency compared with earlier analogs. Notwithstanding, all current editions of the pharmacopeias still do not present any analytical methods for the quantification of SOFO. Thus, rapid, simple, and ecofriendly methods for the routine analysis of commercial formulations of SOFO are desirable. In this study, five accurate methods for the determination of SOFO in pharmaceutical tablets were developed and validated...
January 20, 2017: Journal of AOAC International
Marjan Mahboubifar, Bahram Hemmateenejad, Saeed Yousefinejad
Identification of oil type and its QC are important concerns in food control laboratories. Classifying edible oils thathave not been used (i.e., unheated) with the aid of vibrational spectroscopy has previously been reported. However, the classification of used (i.e., heat-treated) oils needs special attention. The effect of long heating times on the classification of four kinds of edible oils (canola, corn, frying, and sunflower) based on attenuated total reflectance (ATR)-FTIR spectra was surveyed. The sampling was done on the oils during a 36 h heating process (at 170°C)...
January 20, 2017: Journal of AOAC International
Patricia Mattiazzi, Denise Bohrer, Carine Viana, Paulo Cícero do Nascimento, Marlei Veiga, Leandro Machado de Carvalho
A sensitive and accurate method, employing highresolutioncontinuum source atomic absorptionspectrometry, for the determination of antimony(Sb) was developed. Conditions such as pyrolysisand atomization temperatures, the use of chemicalmodifiers, and sample pretreatment were optimizedfor the determination of Sb in pharmaceuticalpreparations and beverages stored in polyethyleneterephthalate (PET) containers. In addition tocontainer analysis, the influence of time of contact,temperature, and content composition on themigration of Sb was investigated...
January 19, 2017: Journal of AOAC International
Pedro H C Franco, Paula R Chellini, Marcone A L Oliveira, Gerson A Pianetti
Tuberculosis is the second most deadly infectiousdisease, surpassed only by HIV/AIDS, and hasresulted in over 1 billion deaths in the last200 years. The World Health Organization estimatesthat in 2014, 9.6 million people were infected bythis disease and 1.5 million had died. First-choicetreatment consists of fixed-dose combinationtablets containing rifampicin, isoniazid,pyrazinamide, and ethambutol hydrochloride(4-FDC). There are pharmacopeial protocolsavailable to test 4-FDC, but they are prolonged,two-step methods...
January 19, 2017: Journal of AOAC International
Dominic Lambert, Arthur Pightling, Emma Griffiths, Gary Van Domselaar, Peter Evans, Sharon Berthelet, Duncan Craig, P Scott Chandry, Robert Stones, Fiona Brinkman, Alexandre Angers-Loustau, Joachim Kreysa, Weida Tong, Burton Blais
The application of new data streams generated from next-generation sequencing (NGS) has been demonstrated for food microbiology, pathogen identification, and illness outbreak detection. The establishment of best practices for data integrity, reproducibility, and traceability will ensure reliable, auditable, and transparent processes underlying food microbiology risk management decisions. We outline general principles to guide the use of NGS data in support of microbiological food safety. Regulatory authorities across intra- and international jurisdictions can leverage this effort to promote the reliability, consistency, and transparency of processes used in the derivation of genomic information for regulatory food safety purposes, and to facilitate interactions and the transfer of information in the interest of public health...
January 19, 2017: Journal of AOAC International
Mamdouh R Rezk, Marwa F Mohamed, Faten Abdelaziz Fathalla, Mostafa A Shehata
A rapid and sensitive HPLC method was developedand validated for selective determination of thehuman growth hormone (hGH) somatropin in thepresence of its deamidated and oxidized degradationproducts. Reversed-phase chromatographywith an acetonitrile and ammonium bicarbonatemobile phase in gradient elution mode was used.A short run time of 15 min allowed rapid andcost-effective analysis, with an average retentiontime of 7.4 min for native hGH, 6.2 min for itsdeamidated form, and 4.3 and 6 min for its oxidizedvariants...
January 19, 2017: Journal of AOAC International
Mônica Cardoso Santos, Sandro Navickiene, Alain Gaujac
Ayahuasca is a potent hallucinogenicbeverage prepared from <em>Banisteriopsis caapi</em>in combination with other psychoactive plants.<em>N</em>,<em>N</em>-dimethyltryptamine, tryptamine, harmine,harmaline, harmalol, and tetrahydroharmine werequantified in ayahuasca samples using a simpleand low-cost method based on SPE and LC with UVdiode-array detection. The experimental variablesthat affect the SPE method, such as type of solidphase and nature of solvent, were optimized...
January 19, 2017: Journal of AOAC International
Yajun Wu, Yange Yang, Mingchang Liu, Bin Wang, Meige Li, Ying Chen
The quality of honey is significantly influencedby floral origin. Mislabeling floral species occursfrequently in beehoney products. To protectconsumers from economic fraud and maintain afair market environment, methods to identify floralspecies in honey are necessary. In our study, realtimePCRs were established, targeting six honeytypes mainly produced in China (canola, Chinesemilkvetch, Chinese chaste tree, locust tree, litchi,and longan). Sensitivity testing on DNA from planttissues exhibited LODs of about 0...
January 16, 2017: Journal of AOAC International
Renata Świderska-Dąbrowska, Krzysztof Piaskowski, Michał J Baran
Analysis and quantification of multiple analytes in complex samples originating from food and environmental matrixes generate large data sets that can be difficult to analyze and interpret. Multivariate analysis and related computation protocols provide an effective platform and enable such problems to be dealt with. This review illustrates the effective application of chemometrics protocols used to improve quantification techniques and the interpretation of raw data from complex samples.
January 13, 2017: Journal of AOAC International
Neha Srivastava, Supriya Kumari, Kishore Nair, Samsul Alam, Syed K Raza
The present paper depicts a novel method based on magnetic SPE (MSPE) for the determination of organophosphorus pesticides (OPs) such as phorate, malathion, and chlorpyrifos in environmental water samples. In this study, C18 functionalized silica-coated core-shell iron oxide magnetic nanoparticles (MNPs) were used as a surface-engineered magnetic sorbent for the selective extraction of pesticides from aqueous samples, followed by GC-MS and GC-tandem MS analysis for confirmative determination of the analytes...
January 12, 2017: Journal of AOAC International
Benjamin J Place
To address community needs, the National Institute of Standards and Technology has developed a candidate Standard Reference Material (SRM) for infant/adult nutritional formula based on milk and whey protein concentrates with isolated soy protein called SRM 1869 Infant/Adult Nutritional Formula. One major component of this candidate SRM is the fatty acid content. In this study, multiple extraction techniques were evaluated to quantify the fatty acids in this new material. Extraction methods that were based on lipid extraction followed by transesterification resulted in lower mass fraction values for all fatty acids than the values measured by methods utilizing in situ transesterification followed by fatty acid methyl ester extraction (ISTE)...
January 12, 2017: Journal of AOAC International
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