bluuebunny/crossref_metadata_2025 huggingface dataset:
Repeatability and Reproducibility of Determination of the Nitrogen Content of Fishmeal by the Combustion (Dumas) Method and Comparison with the Kjeldahl Method: Interlaboratory Study
Authors: Miller Eric L , Bimbo Anthony P , Barlow Stuart M , SHeridan Berni , Burks L B W ,   Collaborators:, Barrins T , Bassompierre M , Brodin A , Brunsgaard G , Henry M , Burks L B , Butler B H , Ellefson W , Gulden J , Henriksen J , Jin L N , Louviere E , Opdebeeck J , Pirozzola P , Schulze C W , Soffia E O , Sorensen H O , Zaldivar J
Published: February 2020

Ten fishmeal samples (hidden duplicates of 4 meals plus 2 high-protein meals as a Youden pair), tryptophan, and nicotinic acid were analyzed by 18 laboratories using the Dumas method. Thirteen of the laboratories also analyzed the same 12 samples using their current Kjeldahl method. Recoveries (± sR) of tryptophan and nicotinic acid were 99.3 ± 1.04 and 98.8 ± 2.11 by Dumas and 97.1 ± 3.03 and 74.6 ± 26.76 by Kjeldahl. The Dumas method gave significantly greater values (P < 0.001) than the Kjeldahl method. For fishmeals, Kjeldahl N 0.989 of Dumas N (P < 0.001). A similar proportionate difference (0.984 of Dumas N) was observed with tryptophan. Most laboratories failed to determine nicotinic acid correctly by Kjeldahl. For fishmeals, the relative standard deviations for repeatability and reproducibility were for Dumas 1.48 and 2.01% and Kjeldahl 1.62 and 2.37%, respectively. A single analysis conducted in 2 laboratories should not differ by more than 5.63% of the mean value when measured by Dumas or by more than 6.64% by Kjeldahl. It is concluded that with fishmeal, Dumas gives a more reliable measure of organic nitrogen than Kjeldahl, and, therefore, Dumas should be the method of choice.
Development of a Simple and Sensitive High-Performance Liquid Chromatography Method for Determination of Glucosamine in Pharmaceutical Formulations
Authors: Nemati Mahboob , Valizadeh Hadi , Ansarin Masood , Ghaderi Farank
Published: February 2020

A column high-performance liquid chromatography (HPLC) method was developed for the determination of glucosamine in dosage forms. Glucosamine was derivatized by addition of a solution containing orthophthaldialdehyde. The HPLC separation was achieved on a Spherimage 80 ODS2 column (250 4 mm id, 5 μm particle size) using an isocratic mobile phase containing phosphate buffermethanol (90 + 10, v/v, pH 6.50) and methanoltetrahydrofuran (97 + 3, v/v) in proportions of 85 + 15 at a flow rate of 1 mL/min, followed by fluorescence detection. The method was validated for specificity, linearity, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ). The detector response for glucosamine HCl was linear over the concentration range of 0.120 μg/mL with a correlation coefficient of 0.9980. The accuracy was between 99.4 and 100.8%. The LOD and the LOQ were 0.009 and 0.027 μg/mL, respectively. The method was applied to determination of glucosamine in solid dosage forms.
A Sensitive Spectrophotometric Method for the Determination of Desloratadine in Tablets
Authors: Çğalar Sena , Öztun Aysel
Published: February 2020

A simple, rapid, and sensitive visible spectrophotometric method was developed, for the first time, for analysis of desloratadine (DE) in tablets. The method is based on the deep-blue colored TCNQ- radical anion formed by interaction of the drug (n-donor) with 7,7,8,8-tetracyanoquinodimethane (TCNQ, π-acceptor) in acetonitrile at ambient temperature. Optimum conditions for the reaction were investigated, absorbances were read at 843 nm, and the linearity range for concentrations of DE was found to be 1.5-13 μg/mL. The reaction product remains stable up to 8 h when kept at room temperature in the dark. The developed method was validated and successfully applied to the determination of DE in tablets. The tablets were also analyzed with a column liquid chromatography method reported in literature. The results from both methods were statistically compared by t- and F-tests. No significant difference was found for the means and standard deviations at 95% confidence level. Accuracy was examined through recovery studies. Being very simple and reliable, the method can be recommended for routine quality control analysis of DE in tablets.
Extractability, Stability, and Allergenicity of Egg White Proteins in Differently Heat-Processed Foods
Authors: Fste Christiane K , Lvberg Kjersti E , Lindvik Helene , Egaas Eliann
Published: February 2020

Hen's egg white protein is a major cause of food allergy, and a considerable number of countries have introduced labeling directions for processed food products. To control compliance with these regulations, analytical assays for the detection of egg in manufactured foods have been developed. In this study, we have tested the performance of 3 commercially available kits for quantitative egg analysis using 6 model heat-processed foods. The 3 assays worked well under standard conditions with soluble egg white proteins, but only the kit using a denaturing-reducing extraction buffer detected egg in complex heat-treated food matrixes. The differently extracted food samples were further used to evaluate the stability and allergenicity of the egg white allergens ovalbumin, ovomucoid, ovotransferrin, and lysozyme with polyclonal anti-egg antibodies and sera of 6 patients with egg allergy. It could be shown that differences in egg protein extractability have a significant impact on the interpretation of study results.
Comparative Evaluation of Two Quantitative Test Methods for Determining the Efficacy of Liquid Sporicides and Sterilants on a Hard Surface: A Precollaborative Study
Authors: Tomasino Stephen F , Hamilton Martin A ,   Collaborators:, Buen M , Fiumara R , Gonzales E , Insalaco J , Rindal M , Schultheiss R , Stahnke P , Verma K , Zandomeni R , Ziemski M
Published: February 2020

Two quantitative carrier-based test methods for determining the efficacy of liquid sporicides and sterilants on a hard surface, the Standard Quantitative Carrier Test MethodASTM E 2111-00 and an adaptation of a quantitative micro-method as reported by Sagripanti and Bonifacino, were compared in this study. The methods were selected based on their desirable characteristics (e.g., well-developed protocol, previous use with spores, fully quantitative, and use of readily available equipment) for testing liquid sporicides and sterilants on a hard surface. In this paper, the Sagripanti-Bonifacino procedure is referred to as the Three Step Method (TSM). AOAC Official Method 966.04 was included in this study as a reference method. Three laboratories participated in the evaluation. Three chemical treatments were tested: (1) 3000 ppm sodium hypochlorite with pH adjusted to 7.0, (2) a hydrogen peroxide/peroxyacetic acid product, and (3) 3000 ppm sodium hypochlorite with pH unadjusted (pH of approximately 10.0). A fourth treatment, 6000 ppm sodium hypochlorite solution with pH adjusted to 7.0, was included only for Method 966.04 as a positive control (high level of efficacy). The contact time was 10 min for all chemical treatments except the 6000 ppm sodium hypochlorite treatment which was tested at 30 min. Each chemical treatment was tested 3 times using each of the methods. Only 2 of the laboratories performed the AOAC method. Method performance was assessed by the within-laboratory variance, between-laboratory variance, and total variance associated with the log reduction (LR) estimates generated by each quantitative method. The quantitative methods performed similarly, and the LR values generated by each method were not statistically different for the 3 treatments evaluated. Based on feedback from the participating laboratories, compared to the TSM, ASTM E 2111-00 was more resource demanding and required more set-up time. The logistical and resource concerns identified for ASTM E 2111-00 were largely associated with the filtration process and counting bacterial colonies on filters. Thus, the TSM was determined to be the most suitable method.
Determination of Low-Level Agricultural Residues in Soft Drinks and Sports Drinks by Liquid Chromatography/Tandem Mass Spectrometry: Single-Laboratory Validation
Authors: Paske Nathan , Berry Bryan , Schmitz John , Sullivan Darryl
Published: February 2020

In this study, sponsored by PepsiCo Inc., a method was validated for measurement of 11 pesticide residues in soft drinks and sports drinks. The pesticide residues determined in this validation were alachlor, atrazine, butachlor, isoproturon, malaoxon, monocrotophos, paraoxon-methyl, phorate, phorate sulfone, phorate sulfoxide, and 2,4-dichlorophenoxyacetic acid (2,4-D) when spiked at 0.100 g/L (1.00 g/L for phorate). Samples were filtered (if particulate matter was present), degassed (if carbonated), and analyzed using liquid chromatography with tandem mass spectrometry. Quantitation was performed with matrix-matched external standard calibration solutions. The standard curve range for this assay was 0.0750 to 10.0 g/L. The calibration curves for all agricultural residues had coefficient of determination (r2) values greater than or equal to 0.9900 with the exception of 2 values that were 0.9285 and 0.8514. Fortification spikes at 0.100 g/L (1.00 g/L for phorate) over the course of 2 days (n = 8 each day) for 3 matrixes (7UP, Gatorade, and Diet Pepsi) yielded average percent recoveries (and percent relative standard deviations) as follows (n = 48): 94.4 (15.2) for alachlor, 98.2 (13.5) for atrazine, 83.1 (41.6) for butachlor, 89.6 (24.5) for isoproturon, 87.9 (24.4) for malaoxon, 96.1 (9.26) for monocrotophos, 101 (25.7) for paraoxon-methyl, 86.6 (20.4) for phorate, 101 (16.5) for phorate sulfone, 93.6 (25.5) for phorate sulfoxide, and 98.2 (6.02) for 2,4-D.
Calculation of Measurement Uncertainty in Quantitative Analysis of Genetically Modified Organisms Using Intermediate PrecisionA Practical Approach
Authors: Žel Jana , Gruden Kristina , Cankar Katarina , tebih Dejan , Blejec Andrej
Published: February 2020

Quantitative characterization of nucleic acids is becoming a frequently used method in routine analysis of biological samples, one use being the detection of genetically modified organisms (GMOs). Measurement uncertainty is an important factor to be considered in these analyses, especially where precise thresholds are set in regulations. Intermediate precision, defined as a measure between repeatability and reproducibility, is a parameter describing the real situation in laboratories dealing with quantitative aspects of molecular biology methods. In this paper, we describe the top-down approach to calculating measurement uncertainty, using intermediate precision, in routine GMO testing of food and feed samples. We illustrate its practicability in defining compliance of results with regulations. The method described is also applicable to other molecular methods for a variety of laboratory diagnostics where quantitative characterization of nucleic acids is needed.
Quantitation and Validation of Fluoroquinolones in Eggs Using Liquid Chromatography/Tandem Mass Spectrometry
Authors: Durden David A , MacPherson Tanya
Published: February 2020

Fluoroquinolone antibiotics are labeled for very limited veterinary use for treatment of some animals and pets, but they are not authorized for food animals in Canada, including egg-producing birds. Because they are approved for other animals, however, fluoroquinolones may appear in eggs through off-labeling or accidental use. This method is capable of quantitating and confirming the presence of 4 fluoroquinolones, ciprofloxacin, danofloxacin, enrofloxacin, and sarafloxacin, over the concentration range 1 to 60 μg/kg (ppb) using 2 internal standards, norfloxacin or lomefloxacin. The compounds are extracted with acidic acetonitrile, isolated using Oasis HLB solid-phase extraction, and quantitated by liquid chromatography/tandem mass spectrometry at 2 transitions. The limits of detection (μg/kg) were evaluated from between-day experiments as: ciprofloxacin, 0.22; danofloxacin (m/z 314), 0.32; enrofloxacin, 0.22; and sarafloxacin, 0.31. The values for the decision limit, CC, were 0.33, 0.36, 0.30, and 0.45 μg/kg, respectively.
Capillary Electrophoretic-Ultraviolet Method for the Separation and Estimation of Zineb, Maneb, and Ferbam in Food Samples
Authors: Aulakh Jatinder Singh , Fekete Agnes , Malik Ashok Kumar , Mahajan Rakesh Kumar , Schmitt-Kopplin Philippe
Published: February 2020

A simple and sensitive capillary electrophoretic method with ultraviolet detection has been developed for the separation and determination of ferbam [iron(III)-dimethyldithiocarbamate], maneb [manganese(II)-ethylenebisdithiocarbamate] and zineb [zinc(II)-ethylenebisdithiocarbamate], in borate buffer, after their acidic decomposition and complexation with CDTA (trans-1,2-diaminocyclohexane-N,N,N,N-tetraacetic acid monohydrate), as CDTA-metal complexes of Fe+3, Mn+2, and Zn+2. The determination is dependent on the pH and the nature of the buffer solutions. In this method, the detection limit (signal-to-noise ratio = 3) is 0.0013, 0.0022, and 0.0023 mM for ferbam, maneb, and zineb, respectively. The relative standard deviation for the analysis of 1 mM of each was found to be 1.5 0.2%. The method was successfully applied for the analysis of red beans and grain samples spiked with ferbam, maneb, and zineb. The applicability of capillary electrophoresis as a useful tool for the simultaneous determination and analysis of ferbam, maneb, and zineb is demonstrated.
Evaluating the Performance of Sampling Plans to Detect Fumonisin B1 in Maize Lots Marketed in Nigeria
Authors: Whitaker Thomas B , Doko M Bruno , Maestroni Britt M , Slate Andrew B , Ogunbanwo Bosede F
Published: February 2020

Fumonisins are toxic and carcinogenic compounds produced by fungi that can be readily found in maize. The establishment of maximum limits for fumonisins requires the development of scientifically based sampling plans to detect fumonisin in maize. As part of an International Atomic Energy Agency effort to assist developing countries to control mycotoxin contamination, a study was conducted to design sampling plans to detect fumonisin in maize produced and marketed in Nigeria. Eighty-six maize lots were sampled according to an experimental protocol in which an average of 17 test samples, 100 g each, were taken from each lot and analyzed for fumonisin B1 by using liquid chromatography. The total variability associated with the fumonisin test procedure was measured for each lot. Regression equations were developed to predict the total variance as a function of fumonisin concentration. The observed fumonisin distribution among the replicated-sample test results was compared with several theoretical distributions, and the negative binomial distribution was selected to model the fumonisin distribution among test results. A computer model was developed by using the variance and distribution information to predict the performance of sampling plan designs to detect fumonisin in maize shipments. The performance of several sampling plan designs was evaluated to demonstrate how to manipulate sample size and accept/reject limits to reduce misclassification of maize lots.
Characterization of Genetically Modified Maize in Weakly Contaminated Seed Batches and Identification of the Origin of the Adventitious Contamination
Authors: Petit Laetitia , Pagny Galle , Baraige Fabienne , Nignol Anne-Ccile , Zhang David , Fach Patrick
Published: February 2020

So far, relatively few genetically modified plants (GMPs) have been planted in the European Union (EU). However, in France, seed batches weakly contaminated by unidentified GM materials have recently been detected among commercial maize seeds (14 seed batches positive out of 447 analyzed). We have developed a 3-step approach to precisely identify the genetic modifications detected in such maize seed batches. First, to isolate GMPs derived from the contaminated seed batches, 10 000 maize seeds of each batch were planted and screened by polymerase chain reaction (PCR) on 100-plant batches, then on 10-plant subbatches, and finally, plant by plant. In a second step, specific identification of the individual GMPs was performed. Finally, to determine the origin of the contamination, each individual GMP was analyzed by simple sequence repeat (SSR) markers. The results showed that all batches were contaminated by few GM seeds, having a GM content <0.1%. Finally, 12 individual GMPs have been isolated from 17 plant pools that were tested positive either for P35-S and/or T-Nos. MON810 and T25 transformation events approved for cultivation in the EU were detected in 7 individual GMPs. The other seed batches were contaminated by genetically modified organisms (GMOs) that are not approved in the EU, including GA21 or the stacking MON810/T25. Presumable identification of T14 was also achieved following sequencing of 1 individual GMP. The data also showed that most of the seed batches were contaminated by several transformation events. Finally, analysis of SSR markers indicated that the contaminations were essentially due to cross-pollination in the seed production process.
Comparison of Four C18 Columns for the Liquid Chromatographic Determination of Deoxynivalenol in Naturally Contaminated Wheat
Authors: Abdel-Aal El-Sayed M , Miah Kaddus , Young J Christopher , Rabalski Iwona
Published: February 2020

Three long and 1 short reversed-phase C18 columns were compared for separation of deoxynivalenol (DON) in extracts of naturally contaminated wheat samples using liquid chromatography with ultraviolet detection and liquid chromatography/mass spectrometry (LC/MS). Among the 3 long columns used, a Symmetry C18 column with an isocratic solvent mixture of wateracetonitrilemethanol (90 + 5 + 5, v/v/v) gave the best separation for DON without interferences from other compounds in the wheat extracts. The Symmetry short (75 mm) column was comparable with the long column (250 mm) in resolving DON but significantly reduced retention time (i.e., 5.8 versus 16.3 min). Increasing the column temperature from 25 to 45C resulted in a further reduction in retention time. Identity of DON in the wheat extracts and standard solutions was confirmed by LC/MS in the positive ion mode, whereby DON appeared with an (M+1)+ ion at a mass-to-charge ratio of 297 plus fragment ions associated with loss of water and/or a 30 atomic mass unit (amu) CH2O fragment. The Symmetry short column was also capable of separating a mixture of the mycotoxins DON, 15-acetyl-DON, nivalenol, and zearalenone by use of a combination of an isocratic and gradient solvent system. The overall method showed high precision, exhibiting a relative standard deviation of 4.8%, limit of detection of 50 ng/g, and limit of quantitation of 165 ng/g. It was significantly correlated with enzyme-linked immunosorbent assay analysis, indicating its appropriateness for safety and quality assurance of wheat and related grains.
Rapid Detection of the Vibrio cholerae ctx Gene in Food Enrichments Using Real-Time Polymerase Chain Reaction
Authors: Fedio Willis , Blackstone George M , Kikuta-Oshima Lynne , Wendakoon Chitra , McGrath Timothy H , DePaola Angelo
Published: February 2020

A real-time polymerase chain reaction (qPCR) assay for the detection of the ctxA gene of toxigenic Vibrio cholerae (Vc) was validated against standard culture techniques. The first experimental phase determined optimal enrichment conditions for detection by culture and qPCR of Vc in shrimp, bottled water, milk, and potato salad. The conditions tested included temperature (35 and 42C), time (6 and 18 h), and effect of shaking (0 and 100 rpm). No definitive trends were found with enrichment temperature or shaking on Vc isolation frequency or detection by qPCR. Generally, Vc was detected by qPCR more frequently than Vc was isolated, but this difference was significant only in the 35C 6 h enrichment without shaking. In the second phase of experiments, shrimp, bottled water, milk, potato salad, and oysters were inoculated with each of 3 toxigenic Vc strains (Latin American O1 strain, an O139 strain, and an O1 strain from the U.S. Gulf Coast) and enriched under static conditions at 42C for 6 and 18 h. Overall, detection frequency of ctx by qPCR was 98 (88/90) and 100 (90/90) after 6 and 18 h enrichments, respectively, while Vc isolation frequency was 87 (78/90) and 83 (75/90) after 6 and 18 h, respectively. Toxigenic Vc can be detected by qPCR within an 8 h work day using the 6 h enrichment procedure, assuming an initial level of at least 12 colony-forming units/g; however, overnight enrichment may be necessary to detect lower levels. These data indicate that the qPCR assay for ctx is a more reliable, sensitive, and rapid alternative to standard Vc culture methods and is applicable to diverse food products.
Delivering Golden Rice to Developing Countries
Authors: Mayer Jorge E
Published: February 2020

Micronutrient deficiencies create a vicious circle of malnutrition, poverty, and economic dependency that we must strive to break. Golden Rice offers a sustainable solution to reduce the prevalence of vitamin A deficiency-related diseases and mortality, a problem that affects the health of millions of children in all developing countries. The technology is based on the reconstitution of the carotenoid biosynthetic pathway by addition of 2 transgenes. The outcome of this high-tech approach will be provided to end users as nutrient-dense rice varieties that are agronomically identical to their own, locally adapted varieties. This intervention has the potential to reach remote rural populations without access to fortification and supplementation programs. As part of our delivery strategy, we are partnering with government and nongovernment, national and international agricultural institutions to navigate through cumbersome and expensive regulatory regimes that affect the release of genetically modified crops, and to create local demand for the biofortified rice varieties.
An Overview of Methods for Assessment of Iron Bioavailability from Foods Nutritionally Enhanced Through Biotechnology
Authors: Cockell Kevin A
Published: February 2020

Iron deficiency and iron deficiency anemia continue to be significant public health problems worldwide. While supplementation and fortification have been viable means to improve iron nutriture of the population in developed countries, they may be less successful in developing regions for a number of reasons, including complexities in distribution and consumer compliance. Biofortification of staple crops, through conventional plant breeding strategies or modern methods of biotechnology, provides an alternative approach that may be more sustainable once initial investments have been made. Three types of biofortification strategies are being essayed, singly or in combination: increasing the total iron content of edible portions of the plant, decreasing the levels of inhibitors of iron absorption, and increasing the levels of factors that enhance iron absorption. Bioavailability is a key concept in iron nutrition, particularly for nonheme iron such as is found in these biofortified foods. An overview is presented of methods for evaluation of iron bioavailability from foods nutritionally enhanced through biotechnology.
Development of Agriculture Biotechnology in Pakistan
Authors: Zafar Yusuf
Published: February 2020

Agriculture plays an important role in the national economy of Pakistan, where most of the rapidly increasing population resides in rural areas and depends on agriculture for subsistence. Biotechnology has considerable potential for promoting the efficiency of crop improvement, food production, and poverty reduction. Use of modern biotechnology started in Pakistan since 1985. Currently, there are 29 biotech centers/institutes in the country. However, few centers have appropriate physical facilities and trained manpower to develop genetically modified (GM) crops. Most of the activities have been on rice and cotton, which are among the top 5 crops of Pakistan. Biotic (virus/bacterial/insect) and abiotic (salt) resistant and quality (male sterility) genes have already been incorporated in some crop plants. Despite acquiring capacity to produce transgenic plants, no GM crops, either produced locally or imported, have been released in the country. Pakistan is signatory to the World Trade Organization, Convention on Biological Diversity, and Cartagena protocols. Several legislations under the Agreement on Trade-Related Aspects of Intellectual Property Rights have been promulgated in the country. National Biosafety Guidelines have been promulgated in April 2005. The Plant Breeders Rights Act, Amendment in Seed Act-1976, and Geographical Indication for Goods are still passing through discussion, evaluation, and analysis phases. Meanwhile, an illegal GM crop (cotton) has already sneaked into farmer's field. Concerted and coordinated efforts are needed among various ministries for implementation of regulation and capacity building for import/export and local handling of GM crops. Pakistan could easily benefit from the experience of Asian countries, especially China and India, where conditions are similar and the agriculture sector is almost like that of Pakistan. Thus, the exchange of information and experiences is important among these nations.
Simultaneous Assay of Olanzapine and Fluoxetine in Tablets by Column High-Performance Liquid Chromatography and High-Performance Thin-Layer Chromatography
Authors: Shah Charmy R , Shah Nehal J , Suhagia Bhanubhai N , Patel Natvarlal M
Published: February 2020

This paper describes validated high-performance liquid chromatographic (LC) and high-performance thin-layer chromatographic (TLC) methods for the simultaneous estimation of olanzapine and fluoxetine in pure powder and tablet formulations. The LC separation was achieved on a Lichrospher 100 RP-180, C18 column (250 mm, 4.0 mm id, 5 m) using 0.05 M potassium dihydrogen phosphate buffer (pH 5.6 adjusted with o-phosphoric acid) acetonitrile (50 + 50, v/v) as the mobile phase at a flow rate of 1 mL/min and ambient temperature. The TLC separation was achieved on aluminum sheets coated with silica gel 60F254 using methanoltoluene (40 + 20, v/v) as the mobile phase. Quantitation was achieved by measuring ultraviolet absorption at 233 nm over the concentration range of 1070 and 40280 g/mL with mean recovery of 99.54 0.89 and 99.73 0.58% for olanzapine and fluoxetine, respectively, by the LC method. Quantitation was achieved by measuring ultraviolet absorption at 233 nm over the concentration range of 100800 and 4003200 ng/spot with mean recovery of 101.53 0.06 and 101.45 0.35% for olanzapine and fluoxetine, respectively, by the TLC method with densitometry. These methods are simple, precise, and sensitive, and they are applicable for simultaneous determination of olanzapine and fluoxetine in tablet formulations.
In Vitro and In Vivo Digestibility of Native Maize Starch Granules Varying in Amylose Contents
Authors: Morita Tatsuya , Ito Yusuke , Brown Ian Lewis , Ando Ryuichi , Kiriyama Shuhachi
Published: February 2020

Digestibility of maize starch granules with different amylose content (AL-0, 22, 54, 68, 80, or 90) was investigated. Measurement of the in vivo resistant starch (RS) content of the starches was performed using surgically prepared ileorectostomized rats. The rats were fed a purified diet containing one of the starches at 652.5 g/kg diet. The in vivo RS content was determined based on the fecal starch excretion. The dietary fiber (DF) value increased as a function of the amylose content in the starch and showed a positive linear correlation with the gelatinization temperature of the granules. In contrast, the in vitro RS content was likely to depend on both the surface area and amylose contents of the starch granules. The maximum in vitro RS content was obtained with AL-68 (54.4). In vivo RS content showed a significant correlation with the amount of in vitro RS but not in respect to the DF detected. The in vivo RS content of AL-68 (43.4) was higher than that found in AL-90 (37.8). A profound gap was observed for AL-54 between the amount of DF (6.4) and RS (in vitro = 46.6 and in vivo = 40.9) present. The results suggest that both in vitro and in vivo digestibility of maize starch is affected by the amylose content and surface area of the granules. The current evaluation suggests that the physiological occurrence of RS from maize starch might be predictable by reference to the in vitro RS value.
Interlaboratory Trial Validation of an Event-Specific Qualitative Polymerase Chain Reaction-Based Detection Method for Genetically Modified RT73 Rapeseed
Authors: Pan Liangwen , Zhang Shuya , Yang Litao , Broll Hermann , Tian Fenghua , Zhang Dabing ,   Collaborators:, Cankar K , Chen Y , Demeke T , Dollard C , Green M , Kok E J , Kui B , Longo F , Rizos K , Su W , Vojvoda J , Žel J , Zhang H
Published: February 2020

The qualitative event-specific polymerase chain reaction detection method of genetically modified (GM) RT73 rapeseed was developed based on the cloned 3 end flanking sequence of RT73 rapeseed integration. The specificity of the method for GM RT73 rapeseed was validated using several different GM rapeseed lines, GM maize lines, GM soybean line, non-GM rapeseed, and other non-GM crops. In this study, the developed method was validated through an interlaboratory study by 12 laboratories from 6 countries. The sensitivity of this method was evaluated using several mixed rapeseed meals with different GM RT73 rapeseed contents from 5.0 to 0.01 prepared by our laboratory. The evaluated results showed that all of the rapeseed endogenous reference high mobility group protein gene (HMG I/Y), figwort mosaic virus 35S (FMV 35S) promoter, and RT73 event-specific fragment could be detected from rapeseed samples at 0.1 (w/w) with a confidence level of more than 95. All results from the 12 laboratories indicated that the developed method could be considered fit for the detection and identification of GM RT73 rapeseed.
Use of Physical and Chemical Properties of Commercial Tomato (Lycopersicon esculentum Mill.) Products forMonitoring Their Quality
Authors: Ordóñez-Santos Luis Eduardo , Arbones Enrique , Vázquez-Oderiz Lourdes , Romero-Rodríguez Angeles , Gómez Julio , López Miguel
Published: February 2020

Eighteen physical and chemical variables were determined in 25 samples of commercial tomato products: total solids, soluble solids, water activity, lycopene, 5-hydroxymethyl-2-furfural, CIELab components (L, a, b, a/b, C, H), total acidity, sodium chloride, wet-weight pulp percentage, alcohol insoluble solids, total pectic substances, ascorbic acid, and pH. In order to maximize the variability of products, samples included crushed tomato, tomato puree, tomato paste, and heavy concentrates and were taken from Italy, France, Spain, Portugal, the United States, Mexico, Colombia, and Chile. Correlation analysis and multidimensional data analysis techniques (principal component analysis and hierarchical classifications) were used to describe the products' variability and to study the relationships among variables. Three variables were selected, with the aim of classifying the collection of samples in a way consistent with the classification obtained with the first principal components. These variables were soluble solids content, the CIELab lightness parameter L, and total pectic substances content.
Interlaboratory Evaluation of Two Enzyme-Linked Immunosorbent Assay Kits for the Determination of Crustacean Protein in Processed Foods
Authors: Sakai Shinobu , Matsuda Rieko , Adachi Reiko , Akiyama Hiroshi , Maitani Tamio , Ohno Yasuo , Oka Michihiro , Abe Akihisa , Seiki Kohsuke , Oda Hiroshi , Shiomi Kazuo , Urisu Atsuo ,   Collaborators:, Arakawa F , Futo S , Haraguchi H , Hirose Y , Hirota M , Iidzuka T , Kan K , Kanayama S , Koike T , Kojima K , Minegishi Y , Mori Y , Nishihara R , Sato H , Yamaguchi A , Yamakawa H , Yasuda K
Published: February 2020

The labeling of foods containing material derived from crustaceans such as shrimp and crab is to become mandatory in Japan because of increases in the number of allergy patients. To ensure proper labeling, 2 novel sandwich enzyme-linked immunosorbent assay (ELISA) kits for the determination of crustacean protein in processed foods, the N kit (Nissui Pharmaceutical Co., Ltd, Ibaraki, Japan) and the M kit (Maruha Nichiro Holdings, Inc., Ibaraki, Japan), have been developed. Five types of model processed foods containing 10 and/or 11.9 g/g crustacean soluble protein were prepared for interlaboratory evaluation of the performance of these kits. The N kit displayed a relatively high level of reproducibility relative standard deviation (interlaboratory precision; 4.08.4 RSDR) and sufficient recovery (6586) for all the model processed foods. The M kit displayed sufficient reproducibility (17.620.5 RSDR) and a reasonably high level of recovery (82103). The repeatability relative standard deviation (RSDr) values regarding the detection of crustacean proteins in the 5 model foods were mostly <5.1 RSDr for the N kit and 9.9 RSDr for the M kit. In conclusion, the results of this interlaboratory evaluation suggest that both these ELISA kits would be very useful for detecting crustacean protein in processed foods.
Determination of Pesticide Residues (>0.5 g/L) in Soft Drinks and Sports Drinks by Gas Chromatography with Mass Spectrometry: Collaborative Study
Authors: Miller Kathleen D , Milne Paul ,   Collaborators:, Berry B , Loo B , Matteini P , Monson K D , Perez R , Rawn T , Reuther J , Rosi F , Summer S , Varelis P
Published: February 2020

A collaborative study was conducted on a method for the measurement of 19 low-level pesticide residues in soft drinks and sports drinks by gas chromatography with mass spectrometry (GC/MS). The pesticide residues determined were 2,4-dichlorodiphenyldichloroethylene (2,4-DDE); 2,4-dichlorodiphenyldichloroethane (2,4-DDD); 4,4-dichlorodiphenyldichloroethylene (4,4-DDE); 2,4-dichlorodiphenyltrichloroethane (2,4-DDT); 4,4-dichlorodiphenyltrichloroethane (4,4-DDT); 4,4-dichlorodiphenyldichloroethane (4,4-DDD); -endosulfan; endosulfan-sulfate; dieldrin; aldrin; ethion; chlorpyrifos; -endosulfan; malathion; methyl-parathion; -hexachlorocyclohexane (-HCH); -HCH; -HCH; and -HCH. Blind fortification solutions containing 4 different levels of pesticide residues (0, 0.1, 0.5, and 1.0 g/L) were provided to 8 collaborating laboratories who used them to create test samples in 6 matrixes (also provided): 2 colas, a diet cola, a clear lemon-lime soft drink, an orange soft drink, and a sports drink. Reproducibility (RSDR) for all 19 pesticide residues in all matrixes ranged from 7 to 151 at the 0.1 g/L level, 11 to 121 at 0.5 g/L, and 14 to 67 at 1.0 g/L. Repeatability (RSDr), applicable to the diet cola and the sports drink, ranged from 1 to 76 for the 19 pesticide residues at the 0.1 g/L level, 9 to 38 at 0.5 g/L, and 9 to 38 at 1.0 g/L. Recoveries for the 19 pesticide residues in allmatrixes ranged from 77 to 645 at the 0.1 g/L level, 60 to 231 at 0.5 g/L, and 61 to 146 at 1.0 g/L. It is recommended that the method be accepted by AOAC as Official First Action with a limit of quantification (LOQ) equal to 0.5 g/L for 4,4-DDT; 2,4-DDT; 2,4-DDD; 4,4-DDE; 4,4-DDD; 2,4-DDE; aldrin; dieldrin; -endosulfan; endosulfan-sulfate; chlorpyrifos; and ethion, and an LOQ equal to 1.0 g/L for -endosulfan; -HCH; -HCH; -HCH; -HCH; methyl-parathion; and malathion.
Determination of Nebivolol and Valsartan in a Fixed-Dose Combination by Liquid Chromatography
Authors: Doshi Ashish S , Bhagwan Sushil S , Mehta Tushar N , Gupta Vinod K , Subaaiah Gunta
Published: February 2020

An accurate and reproducible liquid chromatographic assay method was developed and validated for the determination of nebivolol and valsartan in a capsule formulation. Bufferacetonitrile (55 + 45, v/v) was used for reversed-phase liquid chromatography to determine the contents of nebivolol and valsartan in the combination-capsule dosage form. The method was validated by determining parameters such as specificity, linearity, limits of detection and quantitation, precision, accuracy, and robustness. The method was found to be specific against placebo interference. Linearity was evaluated over the concentration ranges of 28 g/mL for nebivolol and 32128 g/mL for valsartan (the correlation coefficient was 0.9999 for both nebivolol and valsartan). Both the intraday and interday precision values of the system and the method were determined. The accuracy of the method ranged from 100.66 to 102.58 for nebivolol and from 101.17 to 101.85 for valsartan. The proposed method was found to be robust when slight but deliberate changes were made in the analytical conditions. The developed method was found suitable for the assay determination of nebivolol and valsartan in a capsule formulation.
Smart Stability-Indicating Spectrophotometric Methods for Determination of Binary Mixtures Without Prior Separation
Authors: El-Bardicy Mohammad G , Lotfy Hayam M , El-Sayed Mohammad A , El-Tarras Mohammad F
Published: February 2020

Ratio subtraction and isosbestic point methods are 2 innovating spectrophotometric methods used to determine vincamine in the presence of its acid degradation product and a mixture of cinnarizine (CN) and nicergoline (NIC). Linear correlations were obtained in the concentration range from 840 g/mL for vincamine (I), 622 g/mL for CN (II), and 636 g/mL for NIC (III), with mean accuracies 99.72 0.917 for I, 99.91 0.703 for II, and 99.58 0.847 and 99.83 1.039 for III. The ratio subtraction method was utilized for the analysis of laboratory-prepared mixtures containing different ratios of vincamine and its degradation product, and it was valid in the presence of up to 80 degradation product. CN and NIC in synthetic mixtures were analyzed by the 2 proposed methods with the total content of the mixture determined at their respective isosbestic points of 270.2 and 235.8 nm, and the content of CN was determined by the ratio subtraction method. The proposed method was validated and found to be suitable as a stability-indicating assay method for vincamine in pharmaceutical formulations. The standard addition technique was applied to validate the results and to ensure the specificity of the proposed methods.
Development and Validation of a Visible Absorption Densitometry Method for Quantitation of Conessine in Holarrhena antidysenterica (Kurchi)
Authors: Patel Rakesh K , Prajapati Arun M
Published: February 2020

A selective, precise, and accurate high-performance thin-layer chromatographic (HPTLC) method has been proposed for the analysis of conessine in Holarrhena antidysenterica. The method involves visible densitometric evaluation of conessine resolving it by HPTLC on aluminium-based silica gel plates. For visible densitometric evaluation, peak areas were recorded at 520 nm after the resolved bands were derivatized with Dragendorff's reagent and then sprayed with a 10 solution of aqueous sodium nitrite which resulted in reddish brown color. The correlation between the concentration and area was found to be linear within the range of 10 to 60 ng/spot. The method was validated for precision (interday and intraday), repeatability, and accuracy. Mean recovery for conessine was 98.34100.25. The method was applied for the quantitation of conessine in Kurchi. The proposed HPTLC method was found to be precise, specific, sensitive, and accurate and can be used for routine analysis of Kurchi.
Column Reversed-Phase High-Performance Liquid Chromatographic Method for Simultaneous Determination of Rabeprazole Sodium and Domperidone in Combined Tablet Dosage Form
Authors: Sabnis Shweta Sadanand , Dhavale Nilesh Dnvandev , Jadhav Vijay Yeshawantrao , Gandhi Santosh Vilashchand
Published: February 2020

A new, simple column reversed-phase high-performance liquid chromatographic (HPLC) method for simultaneous determination of rabeprazole sodium (RAB) and domperidone (DOM) in a combined tablet dosage form has been developed and validated. Determination was performed using a Jasco HPLC system with a HiQ SiL octadecylsilane (C18) column (250 4.6 mm id), acetonitrile0.1 M ammonium acetate (50 + 50, v/v) mobile phase, and paracetamol as an internal standard. The detection was performed using a UV detector set at 280 nm. The method was validated with respect to linearity, accuracy, precision, and robustness. Beer's law was obeyed in the concentration range of 1.010.0 and 0.55.0 g/mL for RAB and DOM, respectively. The method has been successfully applied for the analysis of drugs in a pharmaceutical formulation.
Gas Chromatographic Analysis of Capsaicin in Gochujang
Authors: Ha Jaeho , Han Kyu-Jai , Kim Ki-Jin , Jeong Seung-Weon
Published: February 2020

A sensitive, precise, and specific gas chromatographic (GC) method was developed for the analysis of capsaicin in Gochujang and validated by comparing with a column high-performance liquid chromatographic (HPLC) method (AOAC 995.03). The method validation parameters yielded good results, including linearity, precision, accuracy, and recovery. The GC separation was performed on a (5 phenyl)-methylpolysiloxane column [length 30 m, internal diameter (id) 250 μm, film thickness 0.25 μm] followed by flame ionization detection. The conditions of temperature programming were initially 220Cfor 1min, rampat5C/minto270C, and hold for 10 min. The recovery of capsaicin in Gochujang was more than 92, and the detection limit and lower determination limit of the GC analysis were 1.0 and 5.0 μg/g, respectively. The calibration graph for capsaicin was linear from 1 to 250 μg/mL for GC and 0.5 to 50 μg/mL for HPLC. The interday and intraday precisions (relative standard deviations) were <4.02.
Determination of 1,4-Dioxane in Household Detergents and Cleaners
Authors: Tanabe Akiko , Kawata Kuniaki
Published: February 2020

A possible human carcinogen, 1,4-dioxane, was investigated as to its concentration levels in household detergents and cleaners currently sold in Japan. A solid-phase extraction combined with stable isotope dilution and gas chromatographic/ mass spectrometric determination was evaluated for the determination of 1,4-dioxane in household products. The evaluation of the method was performed using a recovery study of 1,4-dioxane-d8 from detergent and cleaner samples. The mean overall recovery and relative standard deviation were 78 and 15, respectively. The limit of quantitation was 0.05 mg/kg. This method was satisfactorily applied to the determination of 1,4-dioxane in household products. 1,4-Dioxane was detected in 40 out of the 51 investigated samples. The concentrations ranged from 0.05 to 33 mg/kg, and the mean was 2.7 mg/kg. The mean of the products that included anionic surfactants, i.e., alkylpoly(oxyethylene)sulfates, was 7.2 mg/kg, which was higher than the 0.39 mg/kg mean for the other surfactants. Moreover, the 1,4-dioxane load/person was estimated to be 0.061 mg/day/person in Japan, which was 27 of the load from the domestic effluent.
Determination of Total Soy Isoflavones in Dietary Supplements, Supplement Ingredients, and Soy Foods by High-Performance Liquid Chromatography with Ultraviolet Detection: Collaborative Study
Authors: Collison Mark W
Published: February 2020

An interlaboratory study was conducted to evaluate a method for determining total soy isoflavones in dietary supplements, dietary supplement ingredients, and soy foods. Isoflavones were extracted using aqueous acetonitrile containing a small amount of dimethylsulfoxide (DMSO) and all 12 of the naturally occuring isoflavones in soy were determined by high-performance liquid chromatography (HPLC) with UV detection using apigenin as an internal standard. Fifteen samples (6 pairs of blind duplicates plus 3 additional samples) of soy isoflavone ingredients, soy isoflavone dietary supplements, soy flour, and soy protein products were successfully analyzed by 13 collaborating laboratories in 6 countries. For repeatability, the relative standard deviations (RSDr) ranged from 1.07 for samples containing over 400 mg/g total isoflavones to 3.31 for samples containing 0.87 mg/g total isoflavones, and for reproducibility the RSDR values ranged from 2.29 for samples containing over 400 mg/g total isoflavones to 9.36 for samples containing 0.87 mg/g total isoflavones. HorRat values ranged from 1.00 to 1.62 for all samples containing at least 0.8 mg/g total isoflavones. One sample, containing very low total isoflavones (<0.05 mg/g), gave RSDR values of 175 and a HorRat value of 17.6. This sample was deemed to be below the usable range of the method. The method provides accurate and precise results for analysis of soy isoflavones in dietary supplements and soy foods.
A Comparative Study of First-Derivative Spectrophotometry and Column High-Performance Liquid Chromatography Applied to the Determination of Repaglinide in Tablets and for Dissolution Testing
Authors: AlKhalidi Bashar A , Shtaiwi Majed , AlKhatib Hatim S , Mohammad Mohammad , Bustanji Yasser
Published: February 2020

A fast and reliable method for the determination of repaglinide is highly desirable to support formulation screening and quality control. A first-derivative UV spectroscopic method was developed for the determination of repaglinide in tablet dosage form and for dissolution testing. First-derivative UV absorbance was measured at 253 nm. The developed method was validated for linearity, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ) in comparison to the U.S. Pharmacopeia (USP) column high-performance liquid chromatographic (HPLC) method. The first-derivative UV spectrophotometric method showed excellent linearity [correlation coefficient (r) = 0.9999] in the concentration range of 135 g/mL and precision (relative standard deviation <1.5). The LOD and LOQ were 0.23 and 0.72 g/mL, respectively, and good recoveries were achieved (98101.8). Statistical comparison of results of the first-derivative UV spectrophotometric and the USP HPLC methods using the t-test showed that there was no significant difference between the 2 methods. Additionally, the method was successfully used for the dissolution test of repaglinide and was found to be reliable, simple, fast, and inexpensive.
Determination of Analogs of Sildenafil and Vardenafil in Foods by Column Liquid Chromatography with a Photodiode Array Detector, Mass Spectrometry, and Nuclear Magnetic Resonance Spectrometry
Authors: Choi Dong Mi , Park Sangaeh , Yoon Tae Hyung , Jeong Hye Kyoung , Pyo Jae Sung , Park Janghyun , Kim Deukjoon , Kwon Sung Won
Published: February 2020

Two analogs of sildenafil and vardenafil in food were detected by column liquid chromatography (LC) with a photodiode array detector. They were isolated by preparative LC; their structures were established by mass spectrometry and nuclear magnetic resonance spectrometry. One analog was found to be methisosildenafil (compound A), 5-(5-(3,5-dimethylpiperazin-1-ylsulfonyl)-2-ethoxyphenyl)-1-methyl-3-propyl-1H-pyrazolo[4,3-d]-pyrimidin-7(6H)-one. It is a sildenafil analog with a dimethylpiperazine ring substituted for the methylpiperazine group. The second analog, hydroxyvardenafil (compound B) is reported for the first time in this study. Hydroxyvardenafil's International Union of Pure and Applied Chemistry name is 2-(2-ethoxy-5-(4-(2-hydroxyethyl)-piperazin-1-ylsulfonyl)phenyl)-5-methyl-7-propylimidazo[ 1,5-f][1,2,4]triazin-4(3H)-one. The novel vardenafil analog has a hydroxyl group added to the ethylpiperazine group.