bluuebunny/crossref_metadata_2025 huggingface dataset:
Herbal tea of yellow bitter charm (Eurycoma longifolia Jack.) leaves and its potential analysis for commercial herbs drink
Authors: Supartini  , Maharani R , Fernandes A , Waluyo T K
Published: February 2020

Yellow Bitter Charm (YBC) has been widely known as medicinal plants in Dipterocarps forest ecosystem. Common utilization of YBC is roots and stems, causing problems with its sustainability. In this study, some active compounds contained in YBC leave were identified due to antioxidant of YBC leaf is higher than root and stem. Thus, efficacious diversification products from it leaves as herbal tea was introduced. YBC leaves were taken from Samboja (East Kalimantan), Kotawaringin Timur and Katingan (Central Kalimantan). Chemical compounds showed that YBC leaves contained some important compounds, namely: canthin (anti-cancer), ethanol (aphrodisiac), anti-malaria (eurycomanone), and anti-HIV (quainoid), while other active compounds were saponins, tannins and alkaloids are very good for improving blood circulation. Herbal tea products from YBC leaves are made into 3 flavors, namely: original, jasmine and lime aroma. Organoleptic tests of these products including color, aroma and taste were tested on 58 respondents from different age classes showed that teenager respondents preferred herbal tea with lime aroma, adult respondents preferred jasmine aroma, while elderly respondent was very fond of original due to efficacy considerations. Antioxidant tests on these products proved that aroma additional might cause a decrease in antioxidant activity.
The characteristics of thorny bamboo (Bambusa blumeana) for dissolving pulp
Authors: Aprianis Y , Novriyanti E , Akbar OT
Published: February 2020

This study was aimed to examine the raw material characteristics of thorny bamboo (Bambusa blumeana) from two different origins. Thorny bamboo is one of the raw material for dissolving pulp (rayon pulp). The origins of the bamboos were Agam Regency (West Sumatra Province) (TB1) and Perawang City of Siak Regency (Riau Province) (TB2) that represented highland and lowland, respectively. Bamboos from the two origins were analyzed for their raw material characteristics consisted of growth, chemical contents, fiber dimension and dissolving pulp. The pulping process was carried out in steps as followed: prehydrolyzed, kraft pulping and pulp bleaching. The pre-hydrolysis techniques used acetic acid solution. The kraft condition was active alkali 25% and sulfidity 32%. Meanwhile, the bleaching was conducted in 4 stages. The analysis was done descriptively. Dissolving pulp requires high purity level of alpha-cellulose that would be attained by dissolving other components from the system. The results showed alpha-cellulose of thorny bamboo from Agam (TB1) and Perawang (TB2) were 51.28% and 36.90%, respectively. However, the fiber of TB2 was longer than that of TB1 that 3.22 and 2.62 mm, respectively. The yields pulp kraft of thorny bamboo TB1 and TB2 were 35.25% and 36.28%, respectively. The alpha-cellulose of the thorny bamboo met the standard for dissolving pulp but not the mineral and acid insoluble ash content.
Establishing an evaluation metric to quantify climate change image realism
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Authors: Zhou Sharon , Luccioni Alexandra , Cosne Gautier , Bernstein Michael S , Bengio Yoshua
Published: February 2020

With success on controlled tasks, deep generative models are being increasingly applied to humanitarian applications (Nie et al 2017 Int. Conf. on Medical Image Computing and Computer-Assisted Intervention (Berlin: Springer) pp 417–25, Yanardag et al 2017 Deep Empathy). In this paper, we focus on the evaluation of a conditional generative model that illustrates the consequences of climate change-induced flooding to encourage public interest and awareness on the issue. Because metrics for comparing the realism of different modes in a conditional generative model do not exist, we propose several automated and human-based methods for evaluation. To do this, we adapt several existing metrics and assess the automated metrics against gold standard human evaluation. We find that using Fréchet Inception Distance with embeddings from an intermediary Inception-v3 layer that precedes the auxiliary classifier produces results most correlated with human realism. While insufficient alone to establish a human-correlated automatic evaluation metric, we believe this work begins to bridge the gap between human and automated generative evaluation procedures, and to generate more realistic images of the future consequences of climate change.
Mycophenolate-induced oral ulcers: Case report and literature review
Authors: Asare Kwame , Gatzke Caroline Barone
Published: February 2020

Purpose

A case of mycophenolate mofetil (MMF)–induced oral ulceration in a kidney transplant recipient is reported.

A 54-year-old man who had received a kidney transplant 7 months previously reported to our outpatient clinic with severe oral ulcers with odynophagia and was admitted to the hospital. His maintenance immunosuppressive agents at the time of admission consisted of tacrolimus and mycophenolate. The patient had stable renal function, with all laboratory values within normal ranges. After various alternative etiologies were ruled out, drug-induced oral ulceration was suspected, and the patient’s tacrolimus dose was empirically reduced, resulting in reduction of the trough concentration from 10 ng/mL to 3.3 ng/mL without improvement of the ulceration. Mycophenolate-induced oral ulceration was suspected, and MMF was discontinued. Within 5 days of discontinuation, there was a remarkable improvement in both the size and severity of the ulceration, and the patient was discharged from the hospital. During the next clinic visit (a total of 12 days after MMF was discontinued), the patient’s mouth and esophageal ulcers had completely healed. Six weeks after complete resolution of the ulcer, MMF at a dosage of 250 mg twice daily was initiated; the dosage was subsequently increased to 500 mg twice daily without a recurrence of ulceration.

Conclusion

A 54-year-old man developed oral ulceration after 7 months of MMF therapy. Discontinuation of therapy resulted in prompt resolution of the patient’s ulcers, with no recurrence of ulceration at a lower MMF dose. This is the first case report indicating that mycophenolate-induced ulceration may be dose dependent.
Generalized integration model for improved statistical inference by leveraging external summary data
Authors: Zhang Han , Deng Lu , Schiffman Mark , Qin Jing , Yu Kai
Published: February 2020

Meta-analysis has become a powerful tool for improving inference by gathering evidence from multiple sources. It pools summary-level data from different studies to improve estimation efficiency with the assumption that all participating studies are analysed under the same statistical model. It is challenging to integrate external summary data calculated from different models with a newly conducted internal study in which individual-level data are collected. We develop a novel statistical inference framework that can effectively synthesize internal and external data for the integrative analysis. The new framework is versatile enough to assimilate various types of summary data from multiple sources. We establish asymptotic properties for the proposed procedure and prove that the new estimate is theoretically more efficient than the internal data based maximum likelihood estimate, as well as a recently developed constrained maximum likelihood approach that incorporates the external information. We illustrate an application of our method by evaluating cervical cancer risk using data from a large cervical screening program.
Stereomotion Processing in the Nonhuman Primate Brain
Authors: Héjja-Brichard Yseult , Rima Samy , Rapha Emilie , Durand Jean-Baptiste , Cottereau Benoit R
Published: February 2020

The cortical areas that process disparity-defined motion-in-depth (i.e., cyclopean stereomotion [CSM]) were characterized with functional magnetic resonance imaging (fMRI) in two awake, behaving macaques. The experimental protocol was similar to previous human neuroimaging studies. We contrasted the responses to dynamic random-dot patterns that continuously changed their binocular disparity over time with those to a control condition that shared the same properties, except that the temporal frames were shuffled. A whole-brain voxel-wise analysis revealed that in all four cortical hemispheres, three areas showed consistent sensitivity to CSM. Two of them were localized respectively in the lower bank of the superior temporal sulcus (CSMSTS) and on the neighboring infero-temporal gyrus (CSMITG). The third area was situated in the posterior parietal cortex (CSMPPC). Additional regions of interest-based analyses within retinotopic areas defined in both animals indicated weaker but significant responses to CSM within the MT cluster (most notably in areas MSTv and FST). Altogether, our results are in agreement with previous findings in both human and macaque and suggest that the cortical areas that process CSM are relatively well preserved between the two primate species.
Serum uromodulin and decline of kidney function in older participants of the population-based KORA F4/FF4 study
Authors: Then Cornelia , Then Holger L , Lechner Andreas , Thorand Barbara , Meisinger Christa , Heier Margit , Peters Annette , Koenig Wolfgang , Rathmann Wolfgang , Scherberich Jürgen , Seissler Jochen
Published: February 2020

Background

Uromodulin, a tissue-specific tubular glycoprotein, has recently emerged as a promising biomarker for kidney function and tubular integrity. However, the association of serum uromodulin (sUmod) with renal function decline is still unknown in an older general population.

Methods

We analysed the association of sUmod with the estimated glomerular filtration rate (eGFR) and albuminuria in 1075 participants of the population-based Cooperative Health Research in the Region of Augsburg (KORA) F4 study, ages 62–81 years, at baseline and prospectively after a mean follow-up time of 6.5 years (n = 605) using logistic and linear regression models as well as receiver operating characteristics (ROC) analyses.

Results

Cross-sectionally, sUmod was positively associated with eGFR (β = 0.31 ± 0.02 per higher standard deviation sUmod; P < 0.001) and inversely associated with the urinary albumin:creatinine ratio (β = −0.19 ± 0.04; P < 0.001) after adjustment for sex, age, body mass index, arterial hypertension, prediabetes and diabetes. After multivariable adjustment including baseline eGFR, sUmod was not associated with incident chronic kidney disease (CKD), defined as a decrease in eGFR <60 mL/min/1.73 m2 after 6.5 years of follow-up {odds ratio [OR] 1.02 [95% confidence interval (CI) 0.77–1.36] per higher SD sUmod} but was inversely associated with advanced CKD, defined as incident eGFR <45 mL/min/1.73 m2 [OR 0.64 (95% CI 0.42–0.98)]. The ROC showed no added predictive value of sUmod for kidney function decline in the fully adjusted model.

Conclusions

Higher sUmod was inversely associated with progression to advanced kidney disease but does not provide additional predictive value for the development of CKD in elderly participants of the population-based KORA study.
Lomitapide treatment in a female with homozygous familial hypercholesterolaemia: a case report
Authors: Littmann Karin , Szummer Karolina , Hagström Hannes , Dolapcsiev Karoly , Brinck Jonas , Eriksson Mats
Published: February 2020

Background

Homozygous familial hypercholesterolaemia (FH) is an autosomal-dominant inherited disease presenting with highly elevated low-density lipoprotein cholesterol (LDL-C) levels. Untreated, the patient can develop atherosclerosis and cardiovascular disease already in adolescence. Treatment with statins and ezetimibe is usually not sufficient and LDL apheresis is often required. Lomitapide, an inhibitor of the microsomal triglyceride transfer protein, reduces LDL-C and triglyceride levels and can be used alone or in combination with other therapies in homozygous FH. However, experience with this agent is still limited.

Case summary

We present a young female who was diagnosed with homozygous FH at 6 years of age. She shows a complete lack of normal LDL receptor activity and no cholesterol-lowering effect from statins. The patient was treated with LDL apheresis from 7 years of age. When LDL apheresis treatment extended to twice a week, she began to experience adverse effects, including catheter-related complications, infections, and hospital admissions. When lomitapide treatment was initiated, the frequency of apheresis reduced, the LDL-C levels improved and she has not had any further hospital admissions since. Initially, she suffered from gastrointestinal disturbances. However, after 3 years of treatment with lomitapide 20 mg/day, the patient has not experienced any adverse effects.

Discussion

In this female with homozygous FH adding lomitapide treatment to LDL apheresis has contributed to improved LDL-C levels, a reduction in LDL apheresis sessions and enhanced quality of life. No adverse effects have been reported. These findings suggest that lomitapide can be a drug of choice in patients with homozygous FH.
Impact of flooding on health-related quality of life in England: results from the National Study of Flooding and Health
Authors: Robin Charlotte , Beck Charles , Armstrong Ben , Waite Thomas David , Rubin G James ,   English National Study of Flooding and Health Study Group, Waite Thomas David , Beck Charles R , Amlôt Richard , Kovats Sari , Armstrong Ben , Leonardi Giovanni , Rubin G James , Oliver Isabel , Waite Thomas David , Beck Charles R , Amlôt Richard , Kovats Sari , Armstrong Ben , Leonardi Giovanni , Rubin G James , Oliver Isabel , Oliver Isabel
Published: February 2020

Background

Flooding can have extensive effects on the health and wellbeing of affected communities. The impact of flooding on psychological morbidity has been established; however, the wider impacts of flooding exposure, including on health-related quality of life (HRQoL), have not been described.

Methods

Using data from the English National Study of Flooding and Health cohort, HRQoL 2 and 3 years post-flooding was assessed with the EuroQol Group EQ-5D-5L tool. Associations between exposure groups (flooding and disruption from flooding) and HRQoL were assessed, using ordinal and linear regression, adjusting for a priori confounders.

Results

For both 2 and 3 years post-flooding, the median HRQoL scores were lower in the flooded and disrupted groups, compared with unaffected respondents. A higher proportion of flooded and disrupted respondents reported HRQoL problems in most dimensions of the EQ-5D-5L, compared with unaffected respondents. In year 2, independent associations between exposure to flooding and experiencing anxiety/depression [adjusted odds ratio (aOR) 7.7; 95% CI 4.6–13.5], problems with usual activities (aOR 5.3; 95% CI 2.5–11.9) and pain/discomfort (aOR 2.4; 95% CI 1.5–3.9) were identified. These problems persisted 3 years post-flooding; associations between exposure to flooding and experiencing anxiety/depression (aOR 4.3; 95% CI 2.5–7.7), problems with usual activities (aOR 2.9; 95% CI 1.5–6.1) and pain/discomfort (aOR 2.5; 95% CI 1.5–4.2) were identified.

Conclusions

Exposure to flooding and disruption from flooding significantly reduces HRQoL. These findings extend our knowledge of the impacts of flooding on health, with implications for multi-agency emergency response and recovery plans.
Liquid Chromatographic Determination of Carhenicillin and Ticarcillin in Injectable Dosage Forms
Authors: Mopper Barry
Published: February 2020

A reverse-phase liquid chromatographic method is described for the assay of carbenicillin and ticarcillin in injectable dosage forms. These penicillins were analyzed isocratically on an octadecyl silane column using a mobile phase consisting of acetonitrile-O.OlM potassium phosphate monobasic (12 + 88, v/v) with photometric detection at 225 nm. Propylthiouracil was used as an internal standard. Detector responses were rectilinearly related to concentrations of carbenicillin and ticarcillin in the ranges 40 to 130 ug/mL (r = 0.5987) and 20 to 90 fig/mL (r = 0.9998), respectively. Using the standard additions method, mean recoveries of carbenicillin and ticarcillin from commercial powders for injection were 99.8 and 100.2%, respectively, with a range of 98.1-102.2%. The coefficients of variation (CV) for repeated determinations of total carbenicillin and ticarcillin content in injectables were 0.3 and 0.2%, respectively. A procedure is included for separating the diastereoisomers of both penicillins by ion-pairing reverse-phase liquid chromatography.
Organohalogen Residues in Human Adipose Autopsy Samples from Six Ontario Municipalities
Authors: Williams David T , Lebel Guy L , Junkins Elizabeth
Published: February 2020

Human adipose tissue samples obtained during autopsies in 6 Canadian Great Lakes municipalities were analyzed for chlorobenzenes, polychlorobiphenyls, and organohalogen pesticide residues. The frequency of occurrence and the range and mean for 2JJ organohalogen residues are reported for male and female donors in each municipality. Overall mean residue values in females were significantly higher than those in males for hexachlorobenzen;, β-HCH, p,p'- DDE,»,/» -DDD + o,p'-DDT, and p,p'-DDT. The means and ranges of residue values were similar to those reported in previous Canadian surveys.
Tissue Fluoroacetate Residues in Prairie Dogs Dosed with Low-Level Sodium
Monofluoroacetate
Authors: Hugghins Ernest J , Casper Howard H , David Ward C
Published: February 2020

A total of 83 black-tailed prairie dogs (Cynomys ludovicianus) from South Dakota were subjected to low-level treatment with sodium monofluoroacetate (Compound 1080) in the laboratory (0.01-0.30 mg 1080/kg). The acute oral median lethal dose (LD50) of 1080 administered by oral gavage was established at 0.173 mg/kg. To assay fluoroacetate residues, 8 kinds of tissue from each of 10 prairie dogs dead of low-level 1080 poisoning were analyzed by capillary gas chromatography-mass spectrometry. Of the total of 79 tissues analyzed, 73 contained <100 ppb fluoroacetate, and 67 contained <50 ppb fluoroacetate. To test the effect of secondary poisoning on nontarget species, 8 European ferrets (Mustela furo) were fed ground whole carcasses of prairie dogs dead of low-level 1080 poisoning, with no observable ill effects on the ferrets
Improved Method for Partition of Organophosphate Pesticide Residues on a Solid Phase Partition Column
Authors: Hopper Marvin L
Published: February 2020

A specially modified form of diatomaceous earth was used to develop a solid phase partition column which, with methylene chloride, is used to extract organophosphate pesticides from an aqueous acetone filtrate. This column has proven to be a direct replacement for the time consuming and labor intensive separatory funnel partition of the Luke procedure. Recoveries from the column are quantitative and reproducible for industrial phosphates and a wide range of polar and nonpolar organophosphate pesticides. The column is reusable and convenient and results in a 35-45% savings in time over separatory funnel partition. Neither sulfate columns nor separatory funnels are required, and no emulsions are formed.
Improved Method for Measurement of Dietary Fiber as Non-Starch Polysaccharides in Plant Foods
Authors: Englyst Hans N , Cummings John H
Published: February 2020

A method is described that allows rapid estimation of total, soluble, and insoluble dietary fiber as the non-starch polysaccharides (NSP) in plant foods. It is a modification of an earlier, more complex procedure. Starch is completely removed enzymatically, and NSP is measured as the sum of its constituent sugars released by acid hydrolysis. The sugars may, in turn, be measured by gas chromatography (GC), giving values for individual monosaccharides, or more rapidly by colorimetry. Both GC and colorimetry are suitable for routine measurement of total, soluble, and insoluble dietary fiber in cereals, fruits, and vegetables. Values obtained are not affected by food processing so the dietary fiber content of various processed foods and mixed diets can be calculated simply from knowing the amount in the raw materials. The additional information obtained by GC analysis is valuable in the interpretation of physiological studies and in epidemiology where disease is related to type and amount of dietary fiber.
Pesticide Residues in Milk and Fish Samples Collected from Upper Egypt
Authors: Dogheim Salwa M , Almaz Monir M , Kostandi Samir N , Hegazy Mohamed E
Published: February 2020

In Egypt, buffalo milk is much preferred by consumers over cow's milk, while small catfish and bolti fish are common in the diet of farmers. Samples of buffalo milk, catfish, and bolti fish collected from Beni-Suef Governorate (Upper Egypt) were analyzed for organochlorines and polychlorinated biphenyls. The results obtained by gas chromatography and confirmed by thin-layer chromatographic techniques revealed high amounts of organochlorines in milk; residues were lower but occurred more frequently in fish samples. Pesticide contaminants found most often were HCH isomers including lindane, DDT complex, aldrin and dieldrin, heptachlor and heptachlor epoxide, hexachlorobenzene, and oxychlordane. Polychlorinated biphenyls were not detected in any of the analyzed samples.
Determination and Depletion of Residues in Carbadox, Tylosin, and Virginiamycin in Kidney, Liver, and Muscle of Pigs in Feeding Experiments
Authors: Lauridsen Milter Green , Lund Carl , Jacobsen Merete
Published: February 2020

The results of residue determinations of the growth promotors carbadox, tylosin, and virginiamycin in kidney, liver, and muscle from pigs in feeding experiments are described as well as the analytical methods used. Residues of the carbadox metabolite quinoxaline-2- carboxylic acid were found in liver from pigs fed 20 mg/kg in the diet with a withdrawal time of 30 days. No residues were detected in muscle with zero withdrawal time. The limit of determination was 0.01 mg/kg for both tissues. No residues of virginiamycin and tylosin were found in pigs fed 50 and 40 mg/kg, respectively, in the diet, even with zero withdrawal time. Residues of tylosin of 0.06 mg/kg and below were detected in liver and kidney from pigs fed 200 or 400 mg/kg and slaughtered within 3 h after the last feeding.
Determination of Arsenic and Selenium in Environmental and Agricultural Samples by
Hydride Generation Atomic Absorption Spectrometry
Authors: Hershey J Wilson , Oostdyk Timothy S , Keliher Peter N
Published: February 2020

Agricultural and environmental samples are digested with acid, and arsenic and selenium are determined using hydride generation atomic absorption spectrometry. Interelement interferences are eliminated by high acid concentrations or cation-exchange resins. Agreement with standard reference material is excellent. The technique is also applied to actual samples
Confirmation of Levamisole Residues in Cattle and Swine Livers by Capillary Gas
Chromatography-Electron Impact Mass Spectrometry
Authors: Stout Steven J , Dacunha Adrian R , Tondreau Robert E , Boyd John E
Published: February 2020

Capillary gas chromatography-electron impact mass spectrometry is used to confirm the presence of levamisole in cattle and swine livers at the 0.1 ppm tolerance level. Use of a fused silica capillary column from injector to detector solved chromatographic problems encountered with the analyte. Of the mass specrrometric techniques evaluated, electron impact mass spectrometry provided the most satisfactory data for a confirmatory method. Recoveries from swine and cattle livers fortified at 0.1 ppm averaged 74.9 and 72.7%, respectively, indicating potential utility of this methodology as a quantitative method. Apparent levamisole residues in control livers were less than 0.01 ppm
Analysis of Natural Coloring Matters in Food. III. Applications of Methylation with Diazomethane for the Detection of Lac Color
Authors: Yamada Sadaji , Noda Naoki , Mikami Eiichi , Hayakawa Junko , Yamada Masuo
Published: February 2020

A new method has been proposed for detection of lac color in food. Lac color is a natural color additive derived from a secretion of the insect Coccus Laccae (Laccifer lacca Kerr). It is extracted from food with methanolic oxalic acid and eluted from a column of Amberlite XAD-2 with the same solvent. The fraction containing the lac color is treated with diazomethane to produce 2 reddish-orange markers. The marker species in the reaction mixture are detected by both thinlayer chromatography and reverse-phase liquid chromatography.
Determination of Fluazifop-Butyl and Fluazifop Acid in Soybeans and Soybean Oil Using Liquid Chromatography with Oxidative Amperometric Detection
Authors: Worobey Brian L , Shields J Brian
Published: February 2020

A new method is described for the determination of the herbicide fluazifop-butyl, and its metabolite fluazifop acid, in soybeans and soybean oil as fluazifop acid. Liquid chromatography with amperometric detection (LC/AD) is used to determine fluazifop acid produced from the metabolism or base hydrolysis of fluazifop-butyl in soybeans and soybean oil. These foods were spiked with fluazifopbutyl at 0.05,0.10, and 0.50 ppm and hydrolyzed with 0.2N NaOH in methanol. The hydrolysate (adjusted to pH ≤ 1) is extracted with dichloromethane and the extract is washed with 1.0% NaHC03. The NaHCo3 is acidified to pH ≤ 1 and extracted with dichloromethane; the partitioning is repeated 2 more times. The dichloromethane is removed, mobile phase solvent is added, and aliquots are injected onto a PRP-1 liquid chromatographic column; fluazifop acid is separated from coextracted compounds and detected at an applied potential of + 1.25 V, using an amperometric electrochemical detector in the oxidation mode. Recoveries ranged from 69 ± 6.5 to 101 ± 18% and from 72 ±7.5 to 88 ± 11% for soybeans and soybean oil, respectively. Accuracy of these recoveries was confirmed by use of ^-radiolabeled fluazifop-butyl and by liquid scintillation spectrometry of the 14C-fluazifop acid released.
Ion-Exchange Chromatographic Determination of Hypoglycin A in Canned Ackee Fruit
Authors: Chase G William , Landen William O , Gelbaum Leslie T , Soliman Abdel-Gawad M
Published: February 2020

An ion-exchange chromatographic method was developed to determine hypoglycin A (HG-A) levels in canned ackee fruit by using an amino acid analyzer. HG-A was extracted by homogenizing the sample in 80% alcohol. An isocratic buffer system, consisting of 30% sodium citrate buffer (pH 3.15) and 70% sodium chloride-sodium acetate buffer (pH 7.40) was used to obtain baseline separation between HG-A and the other amino acids. The system can detect HGA levels as low as 4.8 μg/mh. HG-A levels in the edible portion of fruit in 6 cans ranged from 11.0 to 66.5 mg HG-A/can. Recoveries by standard addition averaged 102.5%.
Rapid Determination of Total Cholesterol in Homogenized Milk
Authors: Tsui Ida C
Published: February 2020

A rapid method that is amenable to automation has been developed for the determination of total cholesterol in homogenized milk. The milk sample is saponified in ethanolic KOH in the presence of an internal standard, cholestane. Cholesterol and the internal standard are then isolated by solid-phase extraction on a nonpolar adsorbent and eluted with organic solvent. The evaporated extract is derivatized and analyzed by capillary gas chromatography. Average recovery of cholesterol acetate added to milk prior to saponification was 95%. The average relative standard deviation for repeated analyses was 2%. The limit of detection for this method is 2 mg/100 g. Twenty samples can be analyzed by one analyst in a normal work day if the gas chromatograph is equipped with an autosampler. This method has been compared with a modified AOAC method for the determination of total cholesterol. At a confidence level of 95%, no difference was observed between the 2 methods.
Liquid Chromatographic Determination of Sulfamethazine in Milk
Authors: Weber John D , Smedley Michael D
Published: February 2020

A simple, relatively rapid liquid chromatographic method has been developed for the determination of sulfamethazine (SMZ) in milk at levels in the low ppb range. The method is based on extracting SMZ from milk with chloroform, evaporating the chloroform, dissolving the residues in hexane, extracting into buffers, and chromatographing the buffer solution. The method has been shown to determine levels as low as 5 ppb reliably. Levels ≥7 ppb have been confirmed by gas chromatography/mass spectrometry after derivatization of extracts from fortified, incurred, and shelf milk. Intralaboratory recoveries and percent coefficients of variation are satisfactory. Sulfadimethoxine and sulfaquinoxaline can also be determined by the method. Application of the method to other dairy products is being investigated.
Gravimetric Determination of Ash in Foods: NMKL Collaborative Study
Authors: Mortensen Anna Birthe , Wallin Harriet
Published: February 2020

A gravimetric method for the determination of ash was collaboratively studied in 14 laboratories. The food is ashed at 550 °C to constant weight and the ash is determined by weighing. Seven samples of various food commodities with estimated ash contents varying between low and high (0.07-8.0 g/100 g) were included in the study. The relative standard deviations for reproducibility varied, ranging from 1.0 and 1.3 for ash contents of 7.2 and 8.0 g/100 g, to 11 ± 1% for low ash contents of 0.07 and 0.27 g/100 g.
Diazomethane Derivatization of Sulfamethazine: Formation of Isomeric Products
Authors: Feil Vernon J , Paulson Gaylord D , Lund Anders L
Published: February 2020

Reaction of 4-amino-N-(4,6-dimethyl-2-pyrimidinyl)benzenesulfonamide (sulfamethazine) with diazomethane yields not only 4-amino- N-(4,6-dimethyl-2-pyrimidinyl)-iV-methylbenzenesulfonamide but also 2-(4-aminobenzenesulfonimido)-1,4,6-trimethyl-1,2-dihydropyrimidine. Yields of the latter compound are highly variable and the compound does not show a response to gas chromatography. Thus, results of gas chromatographic determinations of residues of some sulfa drugs in edible meat tissues may be erroneous when diazomethane derivatization is used.
The FDA Pesticides Program: Goals and New Approaches
Authors: Lombardo Pasquale
Published: February 2020

The U.S. Food and Drug Administration (FDA) has carried out a large-scale monitoring program for pesticide residues in foods since the 1960s. The program has evolved continuously as evidenced by a number of recently incorporated modifications and initiatives. Included are greater emphasis on imports; increased and more specific targeting of pesticide/ commodity combinations by geographic area or country; development of individual district sampling plans for domestic and imported foods; expanded use of single residue methods; linkage of information on foreign pesticide usage with food import volumes; development of an analytical methods research plan; and increased cooperative sampling and data exchange with the states. Initiatives to acquire and utilize private sector and other monitoring data are being explored, and aggressive steps are being taken to inform the public of FDA monitoring results in a timely and understandable manner.
Reverse-Phase Liquid Chromatographic Determination of Clioquinol in Cream and Ointment Preparations: Collaborative Study
Authors: Wojtowicz Edward J
Published: February 2020

Seven laboratories participated in a collaborative study to analyze, in duplicate, 2 synthetic formulations and 2 commercial preparations, labeled to contain 3% clioquinol. Clioquinol is determined as its nickel (II) complex by reverse-phase liquid chromatography on a phenylbonded column with a mobile phase of acetonitrile-methanol-water, containing ammonium acetate and nickel chloride. Detection is at 273 nm and diphenylamine is added as an internal standard. Mean recoveries were 99.1 and 101.1%, respectively, for the ointment and cream synthetic preparations and 96.7 and 99.7%, respectively, for the commercial ointment and cream. All results are consistent with the variability of other methods at this concentration range. The method has been approved interim official first action
Gas Chromatographic Determination of Carbetamide Residues in Rape and Soil
Authors: Wu Jia-Lun , Fan De-Fang
Published: February 2020

A gas chromatographic method is described for direct determination of carbetamide residues in rape and soil. Rapeseed, leaves and stem of rape, and soil samples are extracted with acetone and the extracts are cleaned up by coagulation and partition with petroleum ether, followed by extraction with dichloromethane. Carbetamide is determined by gas chromatography using a nitrogen-phosphorus detector. Recovery ranges for rapeseed, leaves and stem of rape, and soil samples fortified with 0.1-10 ppm carbetamide were 91.4-103% [average 97.2 ± 12% (n = 9)], 94.4-102% [98.2 ± 4.4% (n = 12)], 87.9-93.9% [91.2 ± 6.5% (n = 9)1, and 86.7-102% [94.5 ± 4.5% (n = 15)], respectively.
Heavy Metal, pH, and Total Solid Content of Maple Sap and Syrup Produced in Eastern Canada
Authors: Robinson Robin A , Maclean Kenneth S , Macconnell Henry M
Published: February 2020

Maple sap and syrups in eastern Canada were analyzed for pH, total solids, and the heavy metals Cu, Fe, Pb, and Zn. The levels of heavy metals found were within the range normally contained in food and water samples except for Pb. The concentration factor found in reducing sap to syrup did not reflect the same concentration change for the measured parameters. This indicates removal or conversion of heavy metals and organic acids with the sugar sands. There was no statistical difference among provinces with respect to the heavy metal, pH, and total solids content of sap. The only significant difference in syrup occurred with Cu and this appeared to be the result of the processing procedure. As the season progressed, the Cu, Pb, pH, and total solids content of the sap decreased while Zn increased and Fe showed little change. Syrups reflected a similar change. Statistical differences occurred in sap composition among sites within each province.
Use of Deuterated Internal Standards for Quantitation of T-2 and HT-2 Toxins in Human Blood by Tandem Mass Spectrometry
Authors: Pawlosky Robert J , Mirocha Chester J , Wen Y , Abbas Hamed K
Published: February 2020

Deuterated acetyl derivatives (3-trideutero-acetyl-T-2 and 15-trideutero- HT-2) were prepared for use as internal standards for the quantitation of T-2 and HT-2 in blood by tandem mass spectrometry. The method used was multiple reaction monitoring (MRM), which essentially involves the selection of a parent ion for analysis followed by monitoring of the daughter ions generated by collision activated decomposition. The parent ions chosen for the trifluoroacetate derivative of T-2 and HT-2 were m/z+ 478 and 532, respectively. Both parents yield the same daughter ions, i.e., 180, 138, and 121. HT-2 and T-2 were added to blood extracts in amounts ranging from 1 to 20 ppb. The limit of detection is about 0.5 ppb with an effective detection limit of 1.0 ppb in a range of 1-20 ppb. The recovery is about 90%. This method can be used by veterinarians for purposes of diagnostics. It can be used for urine as well as blood.
Liquid Chromatographic Determination of Penicillin V Potassium in Tablets:
Collaborative Study
Authors: Mopper Barry
Published: February 2020

A liquid chromatographic method for the determination of penicillin V potassium in tablets was collaboratively studied by 7 laboratories. The method uses an octadecyl silane reverse-phase column, a mobile phase of acetonitrile-methanol-O.OlM potassium phosphate monobasic (21 + 4 + 75 v/v/v), photometric detection at 225 nm, and sulfadimethoxine as an internal standard. Each collaborator received 6 samples: powdered composites of 2 commercial tablet preparations and 1 synthetic tablet powder mixture, each with blind duplicates. The mean repeatability and reproducibility relative standard deviations for commercial samples were, respectively, 1.10 and 1.46% (250 mg dosage), and 0.84 and 2.82% (500 mg dosage). The average standard recovery from the synthetic formulation was 99.1%, with repeatability and reproducibility relative standard deviations of 1.30 and 3.66%, respectively. The method has been adopted official first action.
Comparison of Colorimetric Monoclonal Enzyme Immunoassay Screening Methods for Detection of Salmonella in Foods
Authors: Curiale Michael S , Joan Klatt Mary , Robison Barbara J , Beck Lisa T
Published: February 2020

A colorimetric enzyme immunoassay (EIA) method for detection of Salmonella in foods has been compared to the AOAC colorimetric monoclonal EIA screening method (986.35,15th ed.; 46.B21-46.B29, 14th ed.). The assays use the same monoclonal antibodies and have similar reactivity toward Salmonella. However, the new assay uses antibody-coated microtiter wells instead of coated magnetic beads to capture Salmonella antigens. Compared with the bead assay, the coated-well assay format requires significantly less time to complete, and was consistently able to detect lower levels of Salmonella In mixed culture. Compared to the standard AOAC culture method for food samples, the plate assay was as productive. No false negatives were obtained by the immunoassay; the false negative rate was 1.1% by the culture method. The rate of agreement between the 2 methods was 99.1 %. The official final action bead assay method for Salmonella in foods, 986.35, and the same assay for use with low-moisture foods, 987.11, have been modified official first action to use antibody-coated microtiter strip-wells
Determination of Total Gossypol in Cottonseed and Cottonseed Meals by Derivative UV Spectrophotometry
Authors: Botsoglou Nickos A , Kufidis Dimitrios C
Published: February 2020

A new method for the determination of total gossypol in cottonseed and cottonseed meals has been developed. The method Involves oxalic acid hydrolysis of the bound gossypol In a methyl ethyl ketone-water azeotrope, partitioning the liberated gossypol Into chloroform, and quantification by 2nd derivative UV spectrophotometry. The 2nd derivative transformation and measurement of the conventional analytical band around 300 nm permits direct quantification of all compounds containing naphthalene nuclei; chromogenic reaction Is not required. The method was tested at concentration levels of total gossypol normally expected for cottonseed and cottonseed meal. Precision and accuracy data suggested an overall relative standard deviation of 4.0% and an overall recovery of 89.5%. Although results for cottonseed and solvent-extracted cottonseed meal analyses were comparable to those obtained by use of American Oil Chemists' Society methods, results were lower for screw-pressed meals. The lower results were attributed to the partial conversion of gossypol, during the cooking process of these meals, to compounds that differ in composition and structure from gossypol and which react with aniline to give false readings
Enzyme-Linked Immunosorbent Assay for Microcystins in Blue-Green Algal Blooms
Authors: Chu Fun S , Huang Xuan , Wei R D
Published: February 2020

A direct competitive enzyme-linked immunosorbent assay (ELISA) for the freshwater blue-green algal toxin mlcrocystln (MCYST) In algae and water was developed. The assay Involves coating antl-MCYST-variant leuclne-arglnine (LR) antibody to the ELISA plate and the use of MCYST-LRperoxidase as the enzyme marker. The linear portion of the standard curve for MCYST in phosphate buffer containing saline (PBS) was 0.5-10.0 ng/mL (25-500 pg/assay). The minimum detection level for MCYST-LR was 0.20 ng/mL (10 pg/assay). Contaminated water could be directly used In the ELISA. The overall analytical recoveries for MCYST-LR added to water at levels of 1-20 ng/mL was 83.4%. For analysis of cellular MCYST, the toxin was first extracted from the algae with 0.1M ammonium bicarbonate, diluted with PBS to less than 0.5 mg dried algae/mL (<5.0 mg wet welght/mL) and directly used in the ELISA. C-18 reverse-phase Sep-Pak cartridges effectively adsorbed MCYST from the toxln-containlng solutions. The toxin could be recovered from the cartridge by elutlng with 60% methanol. Using this approach, an algae extract that was relatively free of MCYST was prepared and was used in a recovery study. The overall analytical recovery of MCYST added to the algae extract In the range of 0.25-20 ppm was 83% with a coefficient of variation of 11.9%. The detection limit for MCYST In dried algae was about 0.25-0.5 pg/g (0.25-0.5 ppm) lyophlllzed algae sample. This method was applied for the analysis of several naturally occurring algal blooms. Limited samples were also analyzed for MYCST by liquid chromatography. ELISA data were in general agreement with those obtainedby liquid chromatography. MCYST concentrations from 0.006 to 2.9 fig/g (6 to 2900 ppb) and from 26 to 5200 /ig/g (26 ppm to 5200 ppm) were found In water and algae (dried weight), respectively
Survey of Residues of Organochlorine Pesticides in Some Marketable Egyptian Fish
Authors: Abdallah M A , Hassan I M , Naguib M M , Abodonia M A
Published: February 2020

One hundred random samples representing 34 species of marketable fish were collected from 8 Egyptian governorates during the period March 1986 to March 1988 and were analyzed for the presence of some organochlorine pesticides. The results showed the predominance of beta-BHC and lindane at maximum levels of 435.30 and 59.00 μg/kg, respectively, for fish samples obtained from Damietta governorate. The corresponding levels of aldrln, and o,p'-DDT were 34.27 and 734.10 μg/kg, respectively, for fish from the Red Sea governorate. gamma-Chlordane, p,p'-DDE, and p.p'-DDT were found in fish from Ismailla governorate at respective maximum levels of 36.17, 234.40, and 57.19 μg/kg. Heptachlor was Identified at 8.50 μg/kg In Port Said governorate fish and o.p'-DDE at 10.59 μg/kg In Suez governorate fish. Mlrex, on the other hand, could not be detected In any of the samples investigated.
In Vitro Assay for Protein Digestibility: Interlaboratory Study
Authors: Mcdonough Frank E , Sarwar Ghulam , Steinke Fred H , Slump Pier , Garcia Salvador , Boisen Sigund
Published: February 2020

True protein digestibilities of 17 protein sources were estimated by 6 laboratories using an in vitro, 3-enzyme digestion system In a pH stat. Samples from animal, vegetable, and mixed food sources were freeze-drled (If not already dried), ground, mixed, and shipped to each collaborator along with a sodium caselnate standard and trypsin, chymotrypsin, and peptidase. The uptake of tltrant during enzymatic digestion was used to calculate estimates of digestibility. Digestibilities ranged from 100% for casein to 89.9% for whole wheat cereal. Mean relative standard deviations for repeatability were 1.4% for rolled oats and < 1 % for the remaining 16 samples. Mean relative standard deviations for reproducibility ranged from 5.0 to 0.8%; values were < 2.5% for 13 of the 17 samples.
Gas Chromatographic Determination of Incurred Dimetridazole Residues in Swine Tissues
Authors: Newkirk David R , Righter Herbert F , Schenck Frank J , Okrasinski Joseph L , Barnes Charlie J
Published: February 2020

A gas chromatographic method for determination of 2-hydroxymethyl- 1-methyl-5-nltrolmldazole (DMZOH), the hydroxy metabolite of dimetridazole, in swine muscle has been developed. The method uses cleanup steps similar to those of an earlier polarographic method. The present method Is capable of quantltatlng levels as low as 2 ppb and detecting less than 1 ppb. Recoveries from 30 control tissues spiked at 1,2, or 4 ppb averaged 80.4%. Performance of the method In Incurred tissue was documented and limited data on the depletion of the metabolite In muscle were generated. The muscle of swine given 150 ppm dimetridazole In feed for 14 days contained less than 1 ppb DMZOH at 12 h withdrawal time.
Atomic Absorption Spectrophotometric Method for Determination of Polydimethylsiloxane Residues in Pineapple Juice: Collaborative Study
Authors: Parker Robert D
Published: February 2020

An atomic absorption spectrophotometric method for determination of polydimethylsiloxane (PDMS) residues In pineapple juice was collaboratively studied by 9 laboratories. PDMS residues are extracted from pineapple Juice with 4- methyl-2-pentanone and the extracted silicone Is measured by atomic absorption spectrophotometry using a nitrous oxide/ acetylene flame. Collaborators analyzed 5 samples Including 1 blind duplicate. Reproducibility relative standard deviations (RSDR) were 13.1% at 31 ppm, 6.9% at 18 ppm, 14.8% at 7.9 ppm, and 16.1 % at 4.9 ppm PDMS. The method has been approved Interim official first action by AOAC.
Optimization of the Determination of Cholesterol in Various Food Matrixes
Authors: Oles Philip , Gates Gloria , Kensinger Seth , Patchell Jacqueline , Schumacher David , Showers Tammy , Silcox Arlene
Published: February 2020

A fractional factorial (Taguchi) experiment was designed to optimize recovery of cholesterol from a baked food matrix. A pretzel sample was chosen for the spiking design experiment. Factors studied Include the alcohol used for saponification, the extraction solvent, hydrolysis conditions, spiking level, use of an antioxidant, and use of hexadecane to prevent physical losses. Of these, hydrolysis conditions and extraction solvent were most Influential In affecting recovery of cholesterol. A method was subsequently validated for determination of cholesterol In cookie, egg, and meat matrixes. The average recovery of spiked cholesterol was 102 ± 5.5% from a total of 29 samples representing these matrixes. The precision (1 slgma) for repetitive analyses of eggs Is about 3%; for sausage, 2%; and for cookies, 3%. The procedure has also been used for determination of cholesterol In pasta, mayonnaise, chocolate, whey, meat, eggs, and potato chips. Spike recoveries for a variety of foods were 93 to 106% with an overall average of 99% and a relative standard deviation of ±4%.
Kjeldahl Method for Determination of Total Nitrogen Content of Milk: Collaborative Study
Authors: Barbano David M , Clark Jenny L , Dunham Chapman E , Flemin Richard J
Published: February 2020

A macro-KJeldahl procedure using a copper catalyst for determination of milk total nitrogen was developed for both traditional and block dlgestor/steam distiller equipment, and the performance was evaluated by collaborative study. In the first trial of the collaborative study, 9 pairs of blind duplicate milk samples were analyzed for total nitrogen and total nitrogen was converted to "protein" by using a factor of 6.38. Protein content of milk samples ranged from 3.086 to 3.610%. In the first trial, sR and R values for the block dlgestors were influenced significantly by protein concentration; 8R and R values were not Influenced by protein concentration for traditional equipment. It was hypothesized that total digestion time for some block dlgestors In the first trial was not sufficient for high protein milk samples. Thus, a second trial was undertaken with boiling time after clearing Increased by 0.5 h. In the second trial, none of the parameters for reproducibility with either type of equipment were Influenced by protein concentration. It was concluded that laboratory-to-laboratory differences In line voltage may require different total digestion times in different laboratories, particularly those using block dlgestors. The Kjeldahl method using a copper catalyst and either traditional or block digestor equipment for determination of milk total nitrogen has been adopted official first action by AOAC to replace method 920.105.