Differential assay of zidovudine and its glucuronide metabolite in serum and urine with a radioimmunoassay kit

1990 ◽  
Vol 36 (6) ◽  
pp. 897-900 ◽  
Author(s):  
S M Tadepalli ◽  
L Puckett ◽  
S Jeal ◽  
L Kanics ◽  
R P Quinn
Keyword(s):  
Inhibitory Concentration ◽  
Serum Samples ◽  
Lower Detection Limit ◽  
Coefficients Of Variation ◽  
Lower Detection ◽  
Before And After ◽  
The Difference ◽  
Glucuronide Metabolite ◽  
Serum And Urine

Abstract We developed an ancillary procedure for the ZDV-Trac RIA (Incstar) to allow simultaneous determination of both zidovudine (3'-azido-3'-deoxythymidine, ZDV, AZT, Retrovir) and its metabolite, the glucuronide of ZDV (3'-azido-3'-deoxy-5'-O-beta-D-glucopyranuronosylthymidine, ZDVG, GAZT), in human serum and urine. Using the ZDV-Trac RIA, we measured ZDV concentrations before and after ZDVG in samples was hydrolyzed to ZDV by beta-glucuronidase (EC 3.2.1.31); ZDVG concentration was calculated as the difference between the two results. This method enables rapid evaluation of a large number of samples with a total turn-around time of 6 h. The lower detection limit of the RIA was 0.27 micrograms/L; the measurements varied linearly with ZDV concentrations from 0.27 to 217 micrograms/L, with the 50% inhibitory concentration being approximately 10 micrograms/L. Analytical recoveries of inhouse serum and urine controls for both ZDV and ZDVG exceeded 90%. Coefficients of variation (CVs) of serum controls were less than 6% for ZDV and less than 11% for ZDVG; for urine controls, CVs for both ZDV and ZDVG were less than 6%. Results for ZDVG concentrations obtained by HPLC and by the ZDV-Trac RIA system compared well: r = 0.978, slope 1.0, for serum samples, and r = 0.993, slope 1.09, for urine samples.

scholarly journals Determination of epinephrine by the Briggs-Rauscher oscillating system using non-equilibrium stationary state

2012 ◽  
Vol 77 (1) ◽  
pp. 95-104 ◽  
Author(s):  
Jinzhang Gao ◽  
Yanjun Liu ◽  
Jie Ren ◽  
Xiaoli Zhang ◽  
Li Ming ◽  
...  
Keyword(s):  
Detection Limit ◽  
Stationary State ◽  
Lower Detection Limit ◽  
Highly Sensitive ◽  
Lower Detection ◽  
Oscillating Reaction ◽  
The Difference ◽  
Foreign Species ◽  
Non Equilibrium

A highly sensitive method for the determination of epinephrine was proposed, which was based on the perturbation of epinephrine to Briggs-Rauscher oscillating system involving malonic acid, Mn2+, H+, IO3 - and H2O2 at non-equilibrium stationary state. The concentration of KIO3 was chosen as a control parameter to find the bifurcation point in this paper. Results showed that a well linear relationship between the difference of potential and the negative logarithm concentrations of epinephrine existed in the range of 1.1?10-7?5.2?10-9 mol L-1 with a lower detection limit of 6.8?10-10mol L-1 and a correlation coefficient of 0.9974. Compared to the classical oscillating reaction, this method has a lower detection limit and wider linear range. The effects of some foreign species, which may possibly be existed with epinephrine, on determination were also investigated. The proposed method has been successfully used to determine the epinephrine both in the serum and adrenaline hydrochloride injection.

Determination of Residual Acrylamide Monomer in Medical Polyacrylamide Hydrogel by HPLC-SPE

2005 ◽  
Vol 288-289 ◽  
pp. 405-408
Author(s):  
Zi Yi Wan ◽  
Ting Fei Xi ◽  
P. Zhao ◽  
Y. Sun ◽  
Z.G. Feng
Keyword(s):  
Detection Limit ◽  
Solid Phase ◽  
Polyacrylamide Hydrogel ◽  
Simple Method ◽  
Lower Detection Limit ◽  
Response Range ◽  
Coefficients Of Variation ◽  
Lower Detection ◽  
Linear Response Range

The polyacrylamide hydrogel (PAMG) has been used in cosmetology in China, Ukraine and Russia since 1990s. Because the monomer acrylamide(AM) used to produce PAMG has been implicated as a potential mutagen and reproductive toxicant[1,2], it is important to accurately determine the amount of residual AM monomer in the PAMG. In this study, a quick, practical and simple method to determine AM is presented with respect to the hydrogel. AM is analysed quantitatively by ODS-3 column with ultraviolet (UV) absorbance detector. AM is separated from interferential component with an aqueous solution of 0.9%NaCl (NS) adjusted at pH~3.7 using hydrochloric acid and then detected at a UV wavelength of 210 nm. The results show that ODS-3 is effective approach for quantifying AM concentrations in PAMG. This method has a lower detection limit of 0.003µg/ml and a linear response range of 0.003 and 0.9 µg/ml (depending on the range required for analysis). Precision studies give coefficients of variation of <3.2%(n=5) for 0.003µg/ml. The recoveries for this method are greater than 90%. When AM content in PAMG is lower than the detection limit of this method, SPE (solid phase extraction) could be used to concentrate AM. In the case, C18 cartridge is used. And the recoveries are about 70% for SPE when AM concentration is lower than ppb.

FRACTIONAL DETERMINATIONS OF URINARY 17-KETOSTEROIDS IN HYPEREMESIS GRAVIDARUM

1962 ◽  
Vol 41 (1) ◽  
pp. 123-128 ◽  
Author(s):  
Pentti A. Järvinen ◽  
Sykkö Pesonen ◽  
Pirkko Väänänen
Keyword(s):  
Hyperemesis Gravidarum ◽  
First Trimester ◽  
Control Group ◽  
Before And After ◽  
Daily Urine ◽  
First Trimester Of Pregnancy ◽  
The Difference

ABSTRACT The fractional determination of 17-ketosteroids in the daily urine was performed in nine cases of hyperemesis gravidarum and in four control cases, in the first trimester of pregnancy both before and after corticotrophin administration. The excretion of total 17-KS is similar in the two groups. Only in the hyperemesis group does the excretion of total 17-KS increase significantly after corticotrophin administration. The fractional determination reveals no difference between the two groups of patients with regard to the values of the fractions U (unidentified 17-KS), A (androsterone) and Rest (11-oxygenated 17-KS). The excretion of dehydroepiandrosterone is significantly higher in the hyperemesis group than in the control group. The excretion of androstanolone seems to be lower in the hyperemesis group than in the control group, but the difference is not statistically significant. The differences in the correlation between dehydroepiandrosterone and androstanolone in the two groups is significant. The high excretion of dehydroepiandrosterone and low excretion of androstanolone in cases of hyperemesis gravidarum is a sign of adrenal dysfunction.

Method for the simultaneous quantification of n-hexane metabolites: application to n-hexane metabolism determination

1996 ◽  
Vol 15 (6) ◽  
pp. 497-503 ◽  
Author(s):  
T. Soriano ◽  
M. Menéndez ◽  
P. Sanz ◽  
M. Repetto
Keyword(s):  
Similar Pattern ◽  
Analytical Procedure ◽  
Daily Basis ◽  
Practical Application ◽  
Simultaneous Quantification ◽  
Exposed Workers ◽  
Before And After ◽  
Time Requirements ◽  
The Difference

1 The described analytical procedure permits the simultaneous determination of the main n-hexane meta bolites in urine. 2-Hexanone, 2-hexanol, 2, 5-hexanediol and 2, 5-hexanedione, were chosen to dose the rats used in this study. All urine samples were collected and analysed on a daily basis, before and after acidic hydrolysis (pH 0.1) by GC/MS. 2-Hexanone, 2, 5-dimethylfurane, γ-valerolac tone and 2, 5-hexanedione were determined before hydro lysis ; 2-hexanol and 2, 5-hexanediol, after hydrolysis; and 5-hydroxy-2-hexanone and 4, 5-dihydroxy-2-hexanone were calculated by the difference between γ-valerolactone and 2, 5-hexanedione with and without hydrolysis, respectively. 2 A metabolic scheme was proposed reflecting the biotransformations undergone by the four compounds assayed. We consider 2, 5-dimethylfurane as a 'true metabolite' because the quantities detected were always greater before hydrolysis. 3 It has been reported that human and rat n-hexane metabolism follow a similar pattern. Therefore, as a practical application and without increasing either sample or time requirements, the simultaneous quantifi cation of the different metabolites and their excretion profile could provide better information about the metabolic situation of exposed workers than the determi nation of 2, 5-hexanedione alone. According to our experimental results, 4, 5-dihydroxy-2-hexanone itself would be a good toxicity indicator.

scholarly journals ANALISIS PERBEDAAN ABNORMAL RETURN DAN TRADING VOLUME ACTIVITY SEBELUM DAN SESUDAH PERISTIWA PENETAPAN UNDANG-UNDANG TAX AMNESTY

2021 ◽  
Vol 10 (3) ◽  
pp. 186-198
Author(s):  
I Komang Wisnu Wardhana ◽  
Hermanto Hermanto ◽  
I Nyoman Nugraha AP
Keyword(s):  
Abnormal Return ◽  
Trading Volume ◽  
Secondary Data ◽  
Volume Activity ◽  
Analytical Technique ◽  
Tax Amnesty ◽  
Average Abnormal Return ◽  
Before And After ◽  
The Difference

The purpose of this study was to determine the difference in the average abnormal return and trading volume activity before and after the enactment of the tax amnesty law on the LQ-45 index. The type of data used in this study is secondary data with data collection techniques using the documentation method. Determination of the sample in this study using purposive sampling method with certain criteria so as to obtain 45 samples. The analytical technique used in this research is paired sample t-test with an observation period of 10 days. The results of this study indicate that: (1) There is no difference in the average abnormal return before and after the enactment of the tax amnesty law. (2) There is no difference in the average trading volume activity before and after the enactment of the tax amnesty law. 

PSV-4 Determination of Deoxynivalenol (DON) Content in Biological Samples as an Indicator of DON Intake in Grower-finisher Pigs

2021 ◽  
Vol 99 (Supplement_1) ◽  
pp. 206-207
Author(s):  
Michael O Wellington ◽  
Michael A Bosompem ◽  
Veronika Nagl ◽  
Daniel A Columbus
Keyword(s):  
Mass Spectrometry ◽  
Biological Samples ◽  
High Performance ◽  
Tandem Mass ◽  
Serum Samples ◽  
Blood Samples ◽  
Swine Diets ◽  
Direct Quantification ◽  
Serum And Urine

Abstract Due to difficulties in obtaining consistent and/or reliable measures of deoxynivalenol (DON) in complete swine diets, we investigated whether measuring DON in biological samples could be used as an indicator of DON ingestion in pigs. In this study, graded levels of DON (1, 3, or 5 ppm) were fed to grower-finisher pigs for a period of 77-d. On d 35 and 77 of the study, urine samples were quantitatively collected over a 24-h period and blood samples were collected between 3 – 4 h after the morning meal on each of those days for serum DON analysis. For direct quantification of DON in urine, high-performance liquid chromatography with tandem mass spectrometry was performed. For serum samples, indirect quantification of DON was performed via enzymatic hydrolysis. We observed that DON content in urine increased linearly as intake of DON increased (Fig.1A; P &lt; 0.05). Analysis of DON in serum follow a similar trend, where serum DON content was increased as DON intake increased (Fig.1B; P &lt; 0.05). An average of 30% of DON ingested was recovered as DON in urine over a 24-h period. In summary, there was a linear relationship between DON intake and DON content in both urine and blood serum, therefore, analyzing DON concentration in serum and urine could be used as a tool to estimate for DON exposure in pigs under controlled conditions.

Pyridine Extraction Method for Determination of Bacitracin in Feeds: Collaborative Evaluation

1979 ◽  
Vol 62 (3) ◽  
pp. 662-670
Author(s):  
Hussein S Ragheb
Keyword(s):  
High Temperature ◽  
Extraction Method ◽  
Main Difficulty ◽  
Coefficients Of Variation ◽  
Significant Difference ◽  
The Difference ◽  
Zinc Bacitracin ◽  
Collaborative Evaluation

Abstract Seventeen laboratories evaluated the pyridine extraction method and neomycin-sensitized agar for the determination of zinc and MD bacitracin in swine and broiler rations at 10 and 100 g/ton. The method was also applied to the analysis of 2 premixes labeled 50 g/lb (MD bacitracin) and 40 g/lb (zinc bacitracin). Bacitracin activity was determined on each of 2 days with 2 dilutions on each day. No significant difference was found between dilutions within a day or between days for each sample. The type of bacitracin or type of feed did not significantly affect results. The difference in results between MD and zinc bacitracin in premixes approached significance. The large coefficients of variation for premixes (ca 13%) and complete feeds (ca 15–30%) indicate operational problems. The main difficulty was evaporation of pyridine. Some laboratories were not able to evaporate it completely, whereas others lost bacitracin activity, probably due to high temperature of drying. The pyridine extraction method as in 42.200 and 42.204 should be discontinued.

scholarly journals Delta-S-Cys-Albumin: A Lab Test that Quantifies Cumulative Exposure of Archived Human Blood Plasma and Serum Samples to Thawed Conditions

2019 ◽  
Vol 18 (10) ◽  
pp. 2121-2137 ◽  
Author(s):  
Joshua W. Jeffs ◽  
Nilojan Jehanathan ◽  
Stephanie M. F. Thibert ◽  
Shadi Ferdosi ◽  
Linda Pham ◽  
...  
Keyword(s):  
Blood Plasma ◽  
Relative Abundance ◽  
Maximum Level ◽  
Cumulative Exposure ◽  
Intact Protein ◽  
Human Blood Plasma ◽  
Serum Samples ◽  
Protein Mass ◽  
Before And After ◽  
The Difference

Exposure of blood plasma/serum (P/S) to thawed conditions (> −30 °C) can produce biomolecular changes that skew measurements of biomarkers within archived patient samples, potentially rendering them unfit for molecular analysis. Because freeze-thaw histories are often poorly documented, objective methods for assessing molecular fitness before analysis are needed. We report a 10-μl, dilute-and-shoot, intact-protein mass spectrometric assay of albumin proteoforms called “ΔS-Cys-Albumin” that quantifies cumulative exposure of archived P/S samples to thawed conditions. The relative abundance of S-cysteinylated (oxidized) albumin in P/S increases inexorably but to a maximum value under 100% when samples are exposed to temperatures > −30 °C. The difference in the relative abundance of S-cysteinylated albumin (S-Cys-Alb) before and after an intentional incubation period that drives this proteoform to its maximum level is denoted as ΔS-Cys-Albumin. ΔS-Cys-Albumin in fully expired samples is zero. The range (mean ± 95% CI) observed for ΔS-Cys-Albumin in fresh cardiac patient P/S (n = 97) was, for plasma 12–29% (20.9 ± 0.75%) and for serum 10–24% (15.5 ± 0.64%). The multireaction rate law that governs S-Cys-Alb formation in P/S was determined and shown to predict the rate of formation of S-Cys-Alb in plasma and serum samples—a step that enables back-calculation of the time at which unknown P/S specimens have been exposed to room temperature. A blind challenge demonstrated that ΔS-Cys-Albumin can detect exposure of groups (n = 6 each) of P/S samples to 23 °C for 2 h, 4 °C for 16 h, or −20 °C for 24 h—and exposure of individual specimens for modestly increased times. An unplanned case study of nominally pristine serum samples collected under NIH-sponsorship demonstrated that empirical evidence is required to ensure accurate knowledge of archived P/S biospecimen storage history.

Improved Spectrophotometric Determination of Cyclopiazonic Acid in Poultry Feed and Corn

1990 ◽  
Vol 73 (2) ◽  
pp. 257-259 ◽  
Author(s):  
Ivan Chang-Yen ◽  
Keshore Bidasee
Keyword(s):  
Detection Limit ◽  
Spectrophotometric Determination ◽  
Spectrophotometric Method ◽  
Cyclopiazonic Acid ◽  
Poultry Feed ◽  
Reaction Conditions ◽  
Lower Detection Limit ◽  
Lower Detection ◽  
Feed Samples

Abstract An improved visible spectrophotometric method has been developed for cyclopiazonic acid in poultry feed and corn. The method Is based on the reaction of cyclopiazonic acid with Ehrlich reagent and detection at 580 nm. Reaction conditions were optimized with respect to reaction and measurement times and acid and Ehrlich reagent concentrations. Calibration curves were linear from 1 to 20 μg cyclopiazonic acid in 3 mL Ehrlich reagent, with a lower detection limit of 0.08 mg/kg for 50 g samples of poultry feed and corn. Recoveries from 50 g samples of poultry feed spiked with cyclopiazonic ranging from 0.16 to 1.20 mg/kg averaged 93.8%. Moldy corn and poultry feed samples analyzed by this method contained between 1 and 4 mg/kg cyclopiazonic acid.

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