New System for Automated Extraction and Simultaneous Determination of Serum Cholesterol and Triglycerides

1975 ◽  
Vol 21 (10) ◽  
pp. 1430-1436 ◽  
Author(s):  
Dorothy F Wease ◽  
Eli S Espinosa ◽  
Yvonne J Anderson
Keyword(s):  
Simultaneous Determination ◽  
Lipid Extraction ◽  
Small Animal ◽  
Correlation Coefficients ◽  
Sample Volume ◽  
Small Sample ◽  
Automated System ◽  
Coefficients Of Variation ◽  
Precision Time

Abstract We describe an automated system for serum lipid extraction and simultaneous determination of cholesterol and triglycerides, with use of continuous-flow equipment. A sample volume of 100 µl of serum is required, and samples are processed at the rate of 20 per hour, which may be increased with slight loss in precision. Time from sample pickup to recorder readout is about 25 min. The system makes use of established colorimetric reactions, and the values obtained agree with ranges currently reported in the literature. Correlation coefficients for results of the automated and manual methods were 0.98 for cholesterol and 0.99 for triglycerides, and the day-to-day coefficients of variation were 1.8% for cholesterol (1 SD = 34 mg/liter) and 3.4% for triglycerides (1 SD = 37 mg/liter). The small sample volume, precision, accuracy, speed, and comparative economy of reagents make this system particularly suitable for multiphasic screening, pediatrics, and small-animal research.

scholarly journals Simultaneous Determination and Stability Studies on Diminazene Diaceturate and Phenazone Using Developed Derivative Spectrophotometric Method

2017 ◽  
Vol 2017 ◽  
pp. 1-6 ◽  
Author(s):  
Ruaa Mohamed Akode ◽  
Shaza Wagiealla Shantier ◽  
Elrasheed Ahmed Gadkariem ◽  
Magdi Awadalla Mohamed
Keyword(s):  
Simultaneous Determination ◽  
Correlation Coefficients ◽  
Degradation Process ◽  
Stability Studies ◽  
Temperature Dependent ◽  
First Order Kinetics ◽  
First Derivative Spectrophotometry ◽  
Aqueous Mixture ◽  
Photo Stability

This work presents UV first derivative spectrophotometry as a precise, accurate, and feasible method for simultaneous determination of diminazene diaceturate and phenazone in bulk and dosage forms. The absorbance values of diminazene diaceturate and phenazone aqueous mixture were obtained at 398 nm and 273 nm, respectively. The developed method was proved to be linear over the concentration ranges (2–10) μg/mL and (2.496–12.48) μg/mL for diminazene diaceturate and phenazone, respectively, with good correlation coefficients (not less than 0.997). The detection and quantitation limits were found to be (LOD = 0.63 and 0.48 μg/mL; LOQ = 1.92 and 1.47 μg/mL, resp.). The developed method was employed for stability studies of both drugs under different stress conditions. Diminazene diaceturate was prone to degrade at acidic pH via first-order kinetics. The degradation process was found to be temperature dependent with an activation energy of 7.48 kcal/mole. Photo-stability was also investigated for this drug.

Design and Performance of a Miniaturized High-Speed Continuous-Flow Analyzer

1974 ◽  
Vol 20 (4) ◽  
pp. 424-427 ◽  
Author(s):  
William E Neeley ◽  
Stephen C Wardlaw ◽  
Helen C Sing
Keyword(s):  
Sample Size ◽  
Continuous Flow ◽  
High Speed ◽  
Clinical Laboratory ◽  
Small Animal ◽  
Sample Volume ◽  
Small Sample ◽  
Reagent Consumption ◽  
And Performance ◽  
Made In

Abstract Design features and performance of a miniaturized high-speed continuous-flow analyzer are described. Special emphasis is made in the design towards a system that is free from the operational and mechanical complexities found in most of today’s advanced systems. Depending on the particular analyses, sample size varies from 3 to 25 µl and reagent consumption is less than 180 µl per sample. Analyses are performed under steady-state conditions at sampling rates of 150 samples per hour with a 2:1 or 3:1 sample-to-wash ratio. The marked reduction in sample size makes the system ideal for microanalyses, especially in the pediatric clinical laboratory, in small animal research, and in any other cases where small sample volume is especially important.

Use of Ten Gram Samples of Corn for Determination of Mycotoxins

1988 ◽  
Vol 71 (1) ◽  
pp. 41-43
Author(s):  
Octave J Francis ◽  
George M Ware ◽  
Allen S Carman ◽  
Gary P Kirschenheuter ◽  
Shia S Kuan
Keyword(s):  
Statistical Tests ◽  
Automated System ◽  
Sample Sizes ◽  
Concentration Variance ◽  
Assay Procedure ◽  
Coefficients Of Variation ◽  
The Mean ◽  
Aflatoxin B ◽  
Test Result

Abstract Data were gathered, during a study on the development of an automated system for the extraction, cleanup, and quantitation of mycotoxins in corn, to determine if it was scientifically sound to reduce the analytical sample size. Five, 10, and 25 g test portions were analyzed and statistically compared with 50 g test portions of the same composites for aflatoxin concentration variance. Statistical tests used to determine whether the 10 and 50 g sample sizes differed significantly showed a satisfactory observed variance ratio (Fobs) of 2.03 for computations of pooled standard deviations; paired f-test values of 0.952, 1.43, and 0.224 were computed for each of the 3 study samples. The results meet acceptable limits, since each sample’s r-test result is less than the published value of the |t|, which is 1.6909 for the test conditions. The null hypothesis is retained since the sample sizes do not give significantly different values for the mean analyte concentration. The percent coefficients of variation (CVs) for all samples tested were within the expected range. In addition, the variance due to sample mixing was evaluated using radioisotopelabeled materials, yielding an acceptable CV of 22.2%. The variance due to the assay procedure was also evaluated and showed an aflatoxin B, recovery of 78.9% and a CV of 11.4%. Results support the original premise that a sufficiently ground and blended sample would produce an analyte variance for a 10 g sample that was statistically comparable with that for a 50 g sample.

scholarly journals Simultaneous Determination of Clopidogrel and Pioglitazone by High Performance Liquid Chromatography in Bulk Drug and Dosage Forms

2013 ◽  
Vol 2 (1) ◽  
pp. 1-9 ◽  
Author(s):  
V Phani Kumar ◽  
Y Sunandamma
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Correlation Coefficients ◽  
High Performance Liquid Chromatographic ◽  
Uv Detection ◽  
Isocratic Elution ◽  
Liquid Chromatographic Method ◽  
Bulk Drug ◽  
Liquid Chromatographic

A high performance liquid chromatographic method with UV detection was developed and validated for simultaneous determination of Pioglitazone and Clopidogrel. Separation was performed on a C18 column by isocratic elution with a mobile phase of Methanol: Acetonitrile: Water (80:10:10) at pH 4.6. The UV detection was set at 230 nm. The method proved to be specific, accurate, precise and linear over the concentration ranges of 20-120ppm for both Pioglitazone and Clopidogrel with correlation coefficients always >0.999 for both drugs. The intra-day and inter-day precision and accuracy were less than 2 for both analytes. DOI: http://dx.doi.org/10.3329/ijpls.v2i1.14580 International Journal of Pharmaceutical and Life Sciences Vol.2(1) 2013: 1-9

Determination of iV-Methylcarbamate Pesticides in Liver by Liquid Chromatography

1989 ◽  
Vol 72 (4) ◽  
pp. 586-592 ◽  
Author(s):  
Sher M Ali
Keyword(s):  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Fluorescence Detection ◽  
Methylene Chloride ◽  
Gel Permeation Chromatography ◽  
Purification Technique ◽  
Coefficients Of Variation ◽  
Gel Permeation ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method using a 2-step purification technique for the simultaneous determination of 10 carbamates in bovine, swine, and duck livers has been developed. Carbamates are extracted from liver samples with methylene chloride. After evaporation, the residues from the extract are dissolved in methylene chloride- cyclohexane (1 + 1) and cleaned up by gel permeation chromatography. The eluate containing carbamate residues is evaporated to dryness, reconstituted in methylene chloride, further purified by passing it through an aminopropyl Bond Elut extraction cartridge, and analyzed by liquid chromatography using post-column derivatization with orthophthalaldehyde and fluorescence detection. Excitation and emission are set at 340 and 418 nm, respectively. Liver samples for beef, pork, and duck were fortified with 5, 10, and 20 ppb of mixed carbamate standards. The average of 10 recoveries of 10 carbamates at all 3 levels of fortification was greater than 80% with coefficients of variation less than 17%.

scholarly journals Seven-Rod Dielectric Sensor for Determination of Soil Moisture in Small Volumes

Proceedings ◽  
2020 ◽  
Vol 15 (1) ◽  
pp. 49
Author(s):  
Justyna Szerement ◽  
Aleksandra Woszczyk ◽  
Agnieszka Szypłowska ◽  
Marcin Kafarski ◽  
Arkadiusz Lewandowski ◽  
...  
Keyword(s):  
Dielectric Permittivity ◽  
Sandy Loam ◽  
Sample Volume ◽  
Small Sample ◽  
Silt Loam ◽  
Frequency Range ◽  
Fem Simulations ◽  
Dielectric Sensor ◽  
Permittivity Spectrum

The paper presents the performance of a seven-rod dielectric probe for determination of soil dielectric permittivity using FEM simulations as well as FDR and TDR measurements. The volume of the sensitivity zone of the tested probe was assessed basing on the simulations and measurement in liquids. The probe was also tested in two soils, sandy loam and silt loam. The obtained results suggested that the seven-rod probe can be used to accurately measure the dielectric permittivity spectrum in a small sample volume of about 8 cm3 in a frequency range from 20 MHz to 200 MHz.

Simultaneous determination of five sex hormones in human serum by radioimmunoassay after chromatography on Lipidex-5000.

1976 ◽  
Vol 22 (1) ◽  
pp. 32-38 ◽  
Author(s):  
D Apter ◽  
O Jánne ◽  
P Karvonen ◽  
R Vihko
Keyword(s):  
Menstrual Cycle ◽  
Human Serum ◽  
Simultaneous Determination ◽  
Sex Hormones ◽  
Oral Contraceptives ◽  
Light Petroleum ◽  
Serum Concentrations ◽  
Coefficients Of Variation ◽  
Normal Men

Abstract We describe a method for determination of pregnenolone, progesterone, 17alpha-hydroxyprogesterone, testosterone, and 5alpha-dihydrotestosterone in 1-2 ml of serum from male or female. Using microcolumns of Lipidex-5000 (hydroxyalkoxypropyl Sephadex, 0.5 g) and light petroleum/chloroform (97/3) as the solvent during chromatography, we resolved these five steroids into four fractions, with pregnenolone and 5alpha-dihydrotestosterone eluting together. By use of selected antibodies, the latter two steroids were also determined specifically. Use of microcolumns allowed minimization of solvent volumes and sample transfers. Consequently, blank values for all the five steroids were negligible. Lowest measureable concentrations (in ng/liter) were: pregnenolone 100, progesterone 25, 17alpha-hydroxyprogesterone 50, testosterone 25, and 5alpha-dihydrotestosterone 25. Intra-assay and inter-assay coefficients of variation ranged from 5 to 9% and 10 to 15%, respectively, for the five steroids. Serum concentrations of these steroids are given for women in the follicular and luteal phases of the menstrual cycle and for women on oral contraceptives of the combination type, as well as for normal men.

scholarly journals LC-MS/MS METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF CARDIAZOL IN HUMAN PLASMA

2019 ◽  
pp. 380-385
Author(s):  
IRYNA DRAPAK ◽  
BORYS ZIMENKOVSKY ◽  
LINA PEREKHODA ◽  
SERGIY KOVALENKO ◽  
Liliya Logoyda
Keyword(s):  
Formic Acid ◽  
Human Plasma ◽  
Method Development ◽  
Accurate Method ◽  
Sample Volume ◽  
Ich Guidelines ◽  
Coefficients Of Variation ◽  
Method Development And Validation ◽  
Development And Validation

Objective: The main purpose of this study was to develop a simple, precise, rapid and accurate method for the quantification of cardiazol in human plasma. Methods: Chromatography was achieved on Discovery C18, 50 × 2.1 mm, 5 μm column. Samples were chromatographed in a gradient mode (eluent A (acetonitrile-water–formic acid, 5: 95: 0.1 v/v), eluent B (acetonitrile–formic acid, 100: 0.1 v/v)). The initial content of the eluent B of 8%, which increases linearly to 1.0 min to 100%, is maintained up to 1.5 min and returned to the original 8% to 1.51 min. The mobile phase was delivered at a flow rate of 0.400 ml/min into the mass spectrometer ESI chamber. The sample volume was 300 μl. Results: The total chromatographic run time was 2.5 min and the elution of cardiazol and IS (difenoconazole) occurred at ~2.15 and 1.98 min, respectively. A linear response function was established at 1-100 ng/ml for cardiazol and difenoconazole in human plasma. The % mean recovery for cardiazol in LQC, MQC and HQC was 102.8 %, 100.3 % and 95.9 %. The lowest concentration with the RSD<20% was taken as LLOQ and was found to be 1.10 ng/ml for cardiazol. The % accuracy of LLOQ samples prepared with the different biological matrix lots was found 109.7 %, which were found within the range of 80.00-120.00 % for the seven different plasma lots. % CV for LLOQ samples was observed as 11.9 %, which are within 20.00% of the acceptance criteria. The within-run coefficients of variation ranged between 0.311 % and 0.601 % for cardiazol. The within-run percentages of nominal concentrations ranged between 99.80 % and 100.41 % for cardiazol. The between-run coefficients of variation ranged between 0.332 % and 0.615 % for cardiazol. The between-run percentages of nominal concentrations ranged between 98.18 % and 101.21 % for cardiazol. Conclusion: A rapid method was developed for simultaneous determination of cardiazol in human plasma. The method was strictly validated according to the ICH guidelines. Acquired results demonstrate that the proposed strategy can be effortlessly and advantageously applied for routine examination of cardiazol in human plasma.

Simultaneous Determination of Sildenafil and Tadalafil in Legal Drugs, Illicit/Counterfeit Drugs, and Wastewater Samples by High-Performance Liquid Chromatography

2016 ◽  
Vol 99 (4) ◽  
pp. 923-928 ◽  
Author(s):  
Ali Kemal Fidan ◽  
Sezgin Bakirdere
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Quantitative Measurement ◽  
Correlation Coefficients ◽  
Wastewater Sample ◽  
Counterfeit Drugs ◽  
Spiking Experiment ◽  
Wastewater Samples ◽  
Erectile Dysfunction Drug

Abstract A sensitive analytical method was developed for the simultaneous determination of sildenafil and tadalafil in legal drugs, illicit/counterfeit drugs, and wastewater samples. Chromatographic separation of two analytes was achieved on a C18 column with a mobile phase including 50 mM phosphate buffer at pH 6.0 and acetonitrile (35 + 65, v/v) at the flow rate of 1.0 mL/min. Analytes were separated from each other in 6 min with high resolution. LOD/LOQ values were calculated as 28/92 ng/mL for sildenafil citrate and 39/129 ng/mL for tadalafil. Calibration plots for both analytes were linear with correlation coefficients &gt;0.9993. A validated method was successfully applied to legal and illicit erectile-dysfunction drug samples consumed in Istanbul, Turkey, and to wastewater samples. Nine different samples were analyzed for qualitative and quantitative measurement of their ingredients, and the results were compared with the values written on the labels of the drugs. The wastewater sample was also analyzed for its sildenafil and tadalafil content. To calculate the recoveries, a spiking experiment was performed and recovery rates for sildenafil and tadalafil were calculated as 101.30 ± 3.43 and 102.68 ± 1.59, respectively.

scholarly journals UPLC–MS/MS simultaneous determination of methamphetamine, amphetamine, morphine, monoacetylmorphine, ketamine, norketamine, MDMA, and MDA in hair

2020 ◽  
Vol 32 (2) ◽  
pp. 145-148 ◽  
Author(s):  
Siyuan Chen ◽  
Jianshe Ma ◽  
Xianqin Wang ◽  
Peiwu Geng
Keyword(s):  
Simultaneous Determination ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Ammonium Hydroxide ◽  
Ultra Performance Liquid Chromatography ◽  
Acetate Solution ◽  
Hair Samples ◽  
Relative Standard

Hair is a stable specimen and has a longer detection window (from weeks to months) than blood and urine. Through the analysis of hair, the long-term information of the drug use of the identified person could be explored. Our work is to establish an ultra-performance liquid chromatography–tandem mass spectroscopy (UPLC–MS/MS) method for simultaneous determination of methamphetamine, amphetamine, morphine, monoacetylmorphine, ketamine, norketamine, 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyamphetamine (MDA) in hair. Methoxyphenamine was used as an internal standard. The chromatographic separation was performed on a UPLC ethylene bridged hybrid (BEH) C18 (2.1 mm × 50 mm, 1.7 μm) column using a mobile phase of acetonitrile–water with 10 mmol/L ammonium acetate solution which containing 0.05% ammonium hydroxide. The multiple reaction monitoring in positive electrospray ionization was used for quantitative determination. The intra-day and inter-day precisions (relative standard deviation [RSD]) were below 15%. The accuracy ranged between 85.5% and 110.4%, the average recovery rate was above 72.9%, and the matrix effect ranged between 92.7% and 109.2%. Standard curves were in the range of 0.05–5.0 ng/mg, and the correlation coefficients were greater than 0.995. The established UPLC–MS/MS method was applied to analyze the hair samples successfully.

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