bluuebunny/crossref_metadata_2025_split huggingface dataset:
Single-Laboratory Validation of the Biosense Direct Competitive Enzyme-Linked Immunosorbent Assay (ELISA) for Determination of Domoic Acid Toxins in Shellfish
Authors: Kleivdal Hans , Kristiansen Sven-Inge , Nilsen Mona V , Briggs Lyn 
Published: July 2020

Abstract
Method validation was conducted for an enzyme-linked immunosorbent assay (ELISA) for the determination of domoic acid (DA) toxins, known to give amnesic shellfish poisoning (ASP) symptoms, in shellfish. The calibration curve range of the assay is approximately 10260 pg/mL, with a dynamic working range for DA toxins in shellfish from 0.01 to at least 250 mg/kg. The ASP ELISA showed no significant cross-reactivity to structural analogs, and proved to be robust to deliberate alterations of the optimal running conditions. The shellfish matrix effects observed with mussels, oysters, and scallops were eliminated by diluting shellfish extracts 1:200 prior to analysis, leading to a limit of detection at 0.003 mg/kg. Thirteen blank shellfish homogenates were spiked with certified mussel material containing DA to levels in the range of 0.125 mg DA/kg, and analyzed in quadruplicate on 3 different days. The relative standard deviation (RSD) under intra-assay repeatability conditions ranged from 6.5 to 13.1%, and under interassay repeatability conditions the RSD ranged from 5.7 to 13.4%, with a mean value of 9.3%. The recoveries ranged from 85.5 to 106.6%, with a mean recovery of 102.2%. A method comparison was conducted with liquid chromatography with ultraviolet detection, using naturally contaminated scallop samples (n = 27) with DA levels at 0244 mg/kg. The overall correlation coefficient was 0.960 and the slope of the regression was 1.218, indicating a good agreement between the methods.
Development of a Capillary Electrophoresis Method for the Enantioselective Estimation of Primaquine in Pharmaceutical Formulations
Authors: Elbashir Abdalla A , Saad Bahruddin , Mohamed Ali Abdussalam Salhin , Saleh Muhammad Idiris 
Published: July 2020

Abstract
A capillary electrophoresis (CE) method has been developed that allows the separation and estimation of primaquine enantiomers using hydroxypropyl--cyclodextrin (HP--CD) as a chiral selector. The influence of chemical and instrumental parameters on the separation, such as type and concentration of CD, buffer concentration, buffer pH, applied voltage, capillary temperature, and injection time, were investigated. Good separation of the racemic mixture of primaquine was achieved using a fused-silica capillary (52.5 cm effective length 50 m id) and a background electrolyte composed of tris-phosphate buffer solution (50 mM, pH 2.5) containing 15 mM HP--CD as a chiral selector. The recommended applied voltage, capillary temperature, and injection time were 15 kV, 25C, and 6 s, respectively. Within-day and interday reproducibility of peak area and migration time gave relative standard deviation values ranging from 1.053.30. Good recoveries (range of 96.8104.9) were obtained from the determination of placebos that were spiked with 0.251.00 mg/L primaquine. The proposed CE method was successfully applied to the assay of primaquine diphosphate in pharmaceutical formulations (tablets).
Adams-Harbertson Protein Precipitation-Based Wine Tannin Method Found Invalid
Authors: Brooks Larry , McCloskey Leo , Mckesson Doug , Sylvan Marshall 
Published: July 2020

Abstract
The poor precision of the Adams-Harbertson wine tannin assay which was proposed for commercial winemaking, thereby creating the real possibility of quality control problems, is documented. The method is a version of the Hagerman and Butler protein precipitation-based tannin method. An extensive invalidation of the assay results with luxury wine data shows that the assay cannot distinguish bottled wine with reasonable accuracy. Five laboratories used Adams-Harbertson to assay 9 replicates each, of 3 bottled wines (n 135) found in California supermarkets, with tannin concentrations of nominally 500 and 1000 ppm by high-performance liquid chromatography (HPLC). Reliability exceeded the 5 industry requirement by nominally 5 times (z-score based on 5 distribution). Coefficient of variation was 27, making the standard deviation range 54 for Pinot Noir, 34 for Merlot, and 44 for Cabernet Sauvignon. Validity exceeded the 100 requirement. Intralaboratory validity recovery was 5563. Interwinery validity was 71178 of the mean for Pinot Noir, 81144 for Merlot, and 83164 for Cabernet Sauvignon. Range as a function of the mean was 89 for Pinot Noir, 55 for Merlot, and 67 for Cabernet Sauvignon. Expect intermethod validity to be nominally 50, i.e., percent recovery to HPLC. These statistically significant errors were predicted by the literature. First-order error is related to the tannin-protein equilibrium constant (Ka), as suggested by the original author, Hagerman, and the protein equivalence point error as suggested by Silber. This does not obviate second-order errors for tannin-protein analytical chemistry. Winemakers using the measurements risk making wines that are relatively more tannic than the measurements report.
Comparison of High-Performance Liquid Chromatographic and Thin-Layer Chromatographic Methods for Determination of Aloin in Herbal Products Containing Aloe vera
Authors: Durón Rosalba Ramírez , Almaguer Luca Ceniceros , Rocha Norma Cecilia Cavazos , Flores Perla Giovanna Silva , Torres Noem Waksman De 
Published: July 2020

Abstract
Aloe vera is a medicinal plant used worldwide to treat a variety of conditions and, as such, has important commercial value. Aloin is a principal component of aloe vera leaves and is used for quality control of products containing it. A semiquantitative thin-layer chromatographic (TLC) method for determining the concentration of aloin in aloe-based products was validated. The results were similar to those of a validated high-performance liquid chromatographic method; therefore, TLC, which is a simple, sensitive, specific, rapid, and cheap method, may be ideal for use in any laboratory for routine analysis of commercial products containing aloe vera.
Aflatoxin Testing in Peanuts: A Proficiency Assessment Scheme for Chinese Analytic Laboratories
Authors: Bao Lei , Bao Zhenmin , Zhang Yibing , Liang Chengzhu , Lu Ning , Liu Xintong , Jin Ying , Ze Pei Jun , Ge Manli , Tian Ling 
Published: July 2020

Abstract
This national assessment program was established by the China National Accreditation Service for Conformity Assessment (CNAS) to evaluate the aflatoxin-testing proficiency of a cross-section of Chinese laboratories. The Shan Dong Inspection and Quarantine Bureau of China conducted the assessment according to ISO 13528:2005 (E) and the International Harmonized Protocol for Proficiency Testing. The 77 laboratories that participated in the study had either been previously accredited by CNAS or were candidates for CNAS accreditation. The analytic samples for this testing scheme were prepared from naturally contaminated peanuts and diluted to approximately 10 g/kg for aflatoxin B1 and 18 g/kg for total aflatoxins. The Ss/p test (with a required result of Ss 0.3p) was used to evaluate the homogeneity of the test samples; sample stability was confirmed with a t-test. The performance of each laboratory was designated by a z-score that was calculated using robust statistics. The robust mean of the participants' results in this study was nearly coincident with the median. A modified Horwitz equation was used to determine the standard deviation. The study compared analytic results obtained by 5 different methods: high-performance liquid chromatography (LC), enzyme-linked immunosorbent assay, thin-layer chromatography, fluorometry, and LC with tandem mass spectrometry. A satisfactory performance rating required z-scores between 2 and 2 for the target analytes. Of the 73 laboratories that reported results for aflatoxin B1, 66 (90.4) performed satisfactorily. Of 32 laboratories that reported total aflatoxins (B1 B2 G1 G2), 30 (93.8) performed satisfactorily. Laboratories whose performance ratings were questionable or unsatisfactory were re-evaluated in a second interlaboratory comparison.
Single-Laboratory Validation of a High-Performance Liquid Chromatographic-Diode Array Detector-Fluorescence Detector/Mass Spectrometric Method for Simultaneous Determination of Water-Soluble Vitamins in Multivitamin Dietary Tablets
Authors: Chen Pei , Atkinson Renata , Wolf Wayne R 
Published: July 2020

Abstract
The purpose of this study was to develop a single-laboratory validated (SLV) method using high-performance liquid chromatography with different detectors diode array detector (DAD); fluorescence detector (FLD); and mass spectrometry (MS) for determination of 7 B-complex vitamins (B1-thiamin, B2-riboflavin, B3-nicotinamide, B6-pyridoxine, B9-folic acid, pantothenic acid, and biotin) and vitamin C in multivitamin/multimineral dietary supplements. The method involves the use of a reversed-phase octadecylsilyl column (4 m, 250 2.0 mm id) and a gradient mobile phase profile. Gradient elution was performed at a flow rate of 0.25 mL/min. After a 5 min isocratic elution at 100 A (0.1 formic acid in water), a linear gradient to 50 A and 50 B (0.1 formic acid in acetonitrile) at 15 min was employed. Detection was performed with a DAD as well as either an FLD or a triple-quadrupole MS detector in the multiple reaction monitoring mode. SLV was performed using Standard Reference Material (SRM) 3280 Multivitamin/Multimineral Tablets, being developed by the National Institute of Standards and Technology, with support by the Office of Dietary Supplements of the National Institutes of Health. Phosphate buffer (10 mM, pH 2.0) extracts of the NIST SRM 3280 were analyzed by the liquid chromatographic (LC)-DAD-FLD/MS method. Following extraction, the method does not require any sample cleanup/preconcentration steps except centrifugation and filtration.
Dipstick Format of an Improved ELISA for On-Site Atrazine Monitoring in Water in Pakistan
Authors: Maqbool Uzma , Anwar-ul-Haq  , Mahboob Sadia 
Published: July 2020

Abstract
A dipstick format was developed for on-site atrazine monitoring in water samples of different origins. It was derived from an in-house-developed ELISA based on polyclonal antibodies that also cross-react with hydroxyatrazine (30%) and terbuthylazine (17%). Test reagents were evaluated for temperature and pH stabilities and rapidity for field applications. Reagents performed well within a temperature range of 20-30°C and were tolerant to alkaline pH (up to 8.5) of the assay buffering system. Tracer incubation time could be reduced to 40 min. Bovine serum albumin addition (1%) in the assay buffer improved assay performance, giving 50% B/B0 (IC50) of 65 ng/L and the lowest LOD of 2 ng/L at 90 B/B0 (IC10). The dipstick ELISA format was standardized on a membrane support. Nylon membrane, positively charged, was superior to PVDF for qualitative or semiquantitative analysis regarding color intensity and stability. Tracer incubation time was further reduced to 30 min with a lowest LOD of 0.1 µg/L. For real sample screening with dipsticks, acceptable results were obtained for water. Significant correlation was found between dipstick and plate ELISA results. Validation using GC with a nitrogen-phosphorus detector and HPLC indicated that dipstick signals in aged water samples, which were mainly due to hydroxyatrazine, were significantly above European Commission regulations of 0.1 µg/L. However, dipsticks were superior, fast, and cost-effective.
Use of Alternative Carrier Materials in AOAC Official MethodSM 2008.05, Efficacy of Liquid Sporicides Against Spores of Bacillus subtilis on a Hard, Nonporous Surface, Quantitative Three-Step Method
Authors: Tomasino Stephen F , Rastogi Vipin K , Wallace Lalena , Smith Lisa S , Hamilton Martin A , Pines Rebecca M 
Published: July 2020

Abstract
The quantitative Three-Step Method (TSM) for testing the efficacy of liquid sporicides against spores of Bacillus subtilis on a hard, nonporous surface (glass) was adopted as AOAC Official MethodSM 2008.05 in May 2008. The TSM uses 5 5 1 mm coupons (carriers) upon which spores have been inoculated and which are introduced into liquid sporicidal agent contained in a microcentrifuge tube. Following exposure of inoculated carriers and neutralization, spores are removed from carriers in three fractions (gentle washing, fraction A; sonication, fraction B; and gentle agitation, fraction C). Liquid from each fraction is serially diluted and plated on a recovery medium for spore enumeration. The counts are summed over the three fractions to provide the density (viable spores per carrier), which is log10-transformed to arrive at the log density. The log reduction is calculated by subtracting the mean log density for treated carriers from the mean log density for control carriers. This paper presents a single-laboratory investigation conducted to evaluate the applicability of using two porous carrier materials (ceramic tile and untreated pine wood) and one alternative nonporous material (stainless steel). Glass carriers were included in the study as the reference material. Inoculated carriers were evaluated against three commercially available liquid sporicides (sodium hypochlorite, a combination of peracetic acid and hydrogen peroxide, and glutaraldehyde), each at two levels of presumed efficacy (medium and high) to provide data for assessing the responsiveness of the TSM. Three coupons of each material were evaluated across three replications at each level; three replications of a control were required. Even though all carriers were inoculated with approximately the same number of spores, the observed counts of recovered spores were consistently higher for the nonporous carriers. For control carriers, the mean log densities for the four materials ranged from 6.63 for wood to 7.14 for steel. The pairwise differences between mean log densities, except for glass minus steel, were statistically significant (P &lt; 0.001). The repeatability standard deviations (Sr) for the mean control log density per test were similar for the four materials, ranging from 0.08 for wood to 0.13 for tile. Spore recovery from the carrier materials ranged from approximately 20 to 70: 20 (pine wood), 40 (ceramic tile), 55 (glass), and 70 (steel). Although the percent spore recovery from pine wood was significantly lower than that from other materials, the performance data indicate that the TSM provides a repeatable and responsive test for determining the efficacy of liquid sporicides on both porous and nonporous materials.
High-Performance Liquid Chromatographic and First Derivative of the Ratio Spectrophotometric Determination of Amlodipine and Valsartan in Their Binary Mixtures
Authors: Kul Dilek , Dogan-Topal Burcu , Kutucu Tugba , Uslu Bengi , Ozkan Sibel A 
Published: July 2020

Abstract
Amlodipine besylate (AML) is a long-acting calcium channel blocker used as an antihypertensive agent. Valsartan (VAL) is also used to treat hypertension, either alone or in combination with other agents. Two-component mixtures of AML and VAL were analyzed by HPLC and the ratio spectra of the first derivative spectrophotometric technique. The spectrophotometric method depends on the first derivative of the ratio-spectra by measurements of the amplitudes at 234.0 nm for VAL and 351.0 nm for AML. Calibration graphs were established for 0.520 g/mL AML and 132 g/mL VAL using the ratio spectra of the first derivative spectrophotometric method. In the HPLC method, an ACE 5 C18 (4.6 150 mm, 5 m) RP column at 30C with the mobile phase methanolacetonitrileNaH2PO4H2O buffer, including 5 mL/L triethylamine and adjusted to pH 3.0 (42 + 18 + 40, v/v/v) at 2.0 mL/min flow rate was used to separate both compounds with detection at 254.0 nm. Linearity was obtained in the concentration range of 0.5500 g/mL for AML and 5.0900 g/mL for VAL. The proposed methods have been extensively validated. These methods allow a number of cost- and time-saving benefits. They were successfully applied to the determination of AML and VAL in synthetic mixtures and in a pharmaceutical dosage form. There was no significant difference between the performance of the proposed methods regarding the mean and SD values. The proposed methods are simple, rapid, and suitable for QC applications.
Development and Validation of an HPTLC Method for Simultaneous Quantitation of Isoorientin, Isovitexin, Orientin, and Vitexin in Bamboo-Leaf Flavonoids
Authors: Wang Jin , Tang Feng , Yue Yongde , Guo Xuefeng , Yao Xi 
Published: July 2020

Abstract
A simple HPTLC method has been developed for the simultaneous determination of isoorientin, isovitexin, orientin, and vitexin, both pure and in commercial samples of bamboo-leaf flavonoids. The flavone C-glycosides, including isoorientin, isovitexin, orientin, and vitexin, were extracted from bamboo-leaf flavonoids with methanol and chromatographed on silica gel 60 plates in an automatic developing chamber with tetrahydrofurantolueneformic acidwater (16 8 2 1, v/v/v/v) mobile phase. Quantitation was obtained with UV detection at 350 nm. Polynomial calibration plots were constructed in the concentration range 2001200 ng/zone for isoorientin, 100600 ng/zone for isovitexin, 160960 ng/zone for orientin, and 30360 ng/zone for vitexin with good correlation coefficients (r ≥ 0.9995). The method was validated for precision (interday and intraday), repeatability, and accuracy. Accuracy of the method was evaluated by a recovery study conducted at three different levels, and the average recovery was found to be 93.95% for isoorientin, 95.30% for isovitexin, 99.79% for orientin, and 100.46% for vitexin. The proposed HPTLC method for estimation of isoorientin, isovitexin, orientin, and vitexin was found to be simple, precise, specific, and accurate and can be used for manufacturing QC of bamboo-leaf flavonoids or for governmental regulatory purposes.
Probability of Detection (POD) as a Statistical Model for the Validation of Qualitative Methods
Authors: Wehling Paul , LaBudde Robert A , Brunelle Sharon L , Nelson Maria T 
Published: July 2020

Abstract
A statistical model is presented for use in validation of qualitative methods. This model, termed Probability of Detection (POD), harmonizes the statistical concepts and parameters between quantitative and qualitative method validation. POD characterizes method response with respect to concentration as a continuous variable. The POD model provides a tool for graphical representation of response curves for qualitative methods. In addition, the model allows comparisons between candidate and reference methods, and provides calculations of repeatability, reproducibility, and laboratory effects from collaborative study data. Single laboratory study and collaborative study examples are given.
Solid-Phase Extraction and Atomic Absorption Spectrometric Determination of Cobalt Using an Octadecyl Bonded Silica Membrane Disk Modified with Cyanex 272
Authors: Karve Manjusha , Gholave Jayram V 
Published: July 2020

Abstract
A simple SPE method for determination of cobalt(II) using a C18 bonded silica membrane disk impregnated with Cyanex 272 has been developed. Cobalt(II) was quantitatively sorbed at pH 6.0 from a sample solution and eluted using 10.0 mL 1.0 M HNO3 prior to its flame atomic absorption spectrometric determination. The influence of eluting agents, the minimum volume and maximum flow rate of the eluent, and interfering ions on cobalt(II) was studied. The method developed for cobalt(II) had an LOD of 1.4 g/L, and a preconcentration factor &gt;200 with an RSD of 0.6. The reusability of the modified disk was for 40 cycles. The method was applied for the determination of cobalt in certified samples, urine, and industrial sludge samples.
PSV-14 Effects of Cordyceps mushroom powder on nursery pig performance
Authors: Richert Jacob A , Palencia Jorge Y P , Chastain Clayton S , Thayer Morgan T , Richert Brian T , Nelssen Jim L 
Published: July 2020

Abstract
The objective of this study was to determine the optimal level of Cordyceps mushroom powder inclusion in diets for nursery pigs. One-hundred sixty crossbred pigs [(Duroc × (York × Landrace)] weaned at 18.8 d of age and weighing an average of 5.94 kg were used in a 35 day, 4 phase growth trial to evaluate Cordyceps mushroom powder as potential alternative to carbadox in nursery pig diets. Pigs were allotted by weight, sex, litter, and assigned to body weight (BW) blocks. Within BW blocks, sex ratios were constant in each pen. Each pen within a BW block was randomly assigned a dietary treatment. Growth performance was analyzed as a RCB design using BW, ADG, ADFI, G:F using GLM procedure of SAS 9.4. There were 5 or 6 pigs/pen and 6 pens/treatment. Five diets were used in the study: a negative diet or a positive control (Carbadox, 55 ppm); 300 or 600 ppm mushroom powder, and a step down treatment (900, 900, 450, 300, 150 ppm mushroom powder during weeks 1 through 5, respectively). At various points of the study, pigs fed the 300 ppm and the step-down mushroom powder treatments tended to have improved (P &lt; 0.10) growth performance compared with those fed the negative control diet. During Phase 4 of the study, pigs fed Carbadox had greater ADG (P &lt; 0.02) and improved feed efficiency (P &lt; 0.09) compared to pigs fed the negative control diet. However, overall data showed that there were no statistical differences among treatments (P &gt; 0.05). In summary, pigs fed 300 ppm mushroom powder or the step-down treatment showed comparable growth performance to pigs fed Carbadox. However, future research is needed under a greater disease challenge to examine mushroom powder’s full potential as an alternative to antibiotics.
Long non-coding RNA PHACTR2-AS1 promotes tongue squamous cell carcinoma metastasis by regulating Snail
Authors: Yuan Fenqian , Miao Zhiguo , Chen Wen , Wu Fanggeng , Wei Chao , Yong Jingkang , Xiao Can 
Published: July 2020

Abstract
Long non-coding RNA is an endogenous non-coding RNA that has currently been proved to be an important player in cancer cell biology. In the present study, we investigated the biological role of PHACTR2-AS1 in tongue squamous cell carcinoma (TSCC). PHACTR2-AS1 was preferentially localized in the cytoplasm, and was notably upregulated in TSCC tissues. High PHACTR2-AS1 was correlated with tumour differentiation, metastatic clinical features, relapse and shortened survival time. Depletion of PHACTR2-AS1 did not affect TSCC cell viability and colony formation ability, whereas substantially inhibited cell migration and invasion in vitro and lung metastasis in vivo. Mechanistically, PHACTR2-AS1 could sponge miR-137 to increase Snail expression, resulting in triggering epithelial–mesenchymal transition process, thereby promoting TSCC cell metastasis. Taken together, our data for the first time elucidate the metastasis-promoting role of PHACTR2-AS1 in TSCC, hinting a new therapeutic target for metastatic TSCC patients.