scholarly journals Determination of Clopidol Residues in Chicken Tissues by Liquid Chromatography: Part I. Optimization of Analytical Conditions and Comparison with AOAC Gas Chromatography Method

2001 ◽  
Vol 84 (5) ◽  
pp. 1337-1342 ◽  
Author(s):  
Guo-Fang Pang ◽  
Yan-Zhong Cao ◽  
Chun-Lin Fan ◽  
Jin-Jie Zhang ◽  
Xue-Min Li ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Chromatography Method ◽  
Anion Exchange Column ◽  
Chicken Tissues ◽  
Relative Standard ◽  
Liver And Kidney ◽  
Gas Chromatographic Method ◽  
Liquid Chromatographic

Abstract A simple and specific liquid chromatographic method was developed for determination of clopidol in chicken tissues. Samples were extracted with acetonitrile. The extracts were cleaned up on an alumina column and an anion exchange column. The clopidol was separated on a column (30 cm × 3.9 mm) of μBondapak C18 (10 μm) by using acetonitrile–water (20 + 80, v/v) as mobile phase, and determined quantitatively at 270 nm. Recoveries were 86.0–97.6%, with relative standard deviations of 2.14–9.42% at 0.010–2.0 mg/kg from 4 spiked matrixes of chicken muscle, egg, liver, and kidney. The limit of detection was 0.005 mg/kg. Compared with the modified AOAC gas chromatographic method, the present method is simple and fast to operate. Its results are accurate and reliable, making it favorable for environmental protection and meeting requirements for human safety. Thus, it is suitable for routine analysis of large quantities of samples.

scholarly journals Determination of residual solvents in paclitaxel by headspace gas chromatography

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Khaleel Noorbasha ◽  
Abdul Rahaman Shaik
Keyword(s):  
Ethyl Acetate ◽  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Limit Of Detection ◽  
Good Resolution ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Gas Chromatographic Method ◽  
Ethyl Amine

Abstract Background A simple and sensitive gas chromatographic method was developed and validated for the simultaneous determination of methanol, ethanol, acetone, isopropyl alcohol, dichloromethane, N-hexane, ethyl acetate, tetrahydrofuran, and N,N-diisopropyl ethyl amine in Paclitaxel. A chromatographic separation was done on DB-624 column, 30 m length × 0.53 mm ID, and film thickness 3 μm, using a flame ionization detector (FID) with gradient column oven temperature program. The injection was carried out in split mode, with a split ratio of 5:1. A mixture of N-methyl-2-pyrrolidinone (contains 1% piperazine) and water in the ratio of 80:20 (v/v) was selected as a diluent to obtain good sensitivity along with the recovery. Results The developed gas chromatographic method offers symmetric peak shape, good resolution of more than 2.0 between the solvent peaks, and the relative standard deviation for replicate injections of all the solvents were found to be not more than 15.0% with reasonable retention time for all the solvents. The limit of detection for methanol, ethanol, acetone, isopropyl alcohol, dichloromethane, N-hexane, ethyl acetate, tetrahydrofuran, and N,N-diisopropyl ethyl amine was found to be 304.69 ppm, 497.98 ppm, 498.99 ppm, 504.49 ppm, 61.81 ppm, 30.07 ppm, 505 ppm, 73.05 ppm, and 2.09 ppm, respectively. Limit of quantitation of methanol, ethanol, acetone, isopropyl alcohol, dichloromethane, N-hexane, ethyl acetate, tetrahydrofuran, and N,N-diisopropyl ethyl amine was found to be 89.62 ppm, 146.47 ppm, 146.76 ppm, 148.38 ppm, 18.18 ppm, 8.84 ppm, 148.53 ppm, 21.49 ppm, and 0.62 ppm, respectively. Precision was found to be satisfactory. Linear in the range of LOQ to 150% level for all the solvents, and accuracy along with robustness, is performed, and acceptable results were obtained. Conclusion The proposed method was demonstrated to be simple, sensitive, specific, linear, precise, accurate, and robust, hence can be used to determine the residual organic solvents in Paclitaxel drug substance and drug product.

Determination of carbamazepine in blood or plasma by high-pressure liquid chromatography.

1976 ◽  
Vol 22 (7) ◽  
pp. 1070-1072 ◽  
Author(s):  
P M Kabra ◽  
L J Marton
Keyword(s):  
High Pressure ◽  
Chromatographic Method ◽  
Limit Of Detection ◽  
Internal Standard ◽  
High Pressure Liquid Chromatographic ◽  
Blood Constituents ◽  
Liquid Chromatographic Method ◽  
Gas Chromatographic Method ◽  
Liquid Chromatographic

Abstract We described a sensitive and precise high-pressure liquid-chromatographic method in which 5-(p-methylphenyl)-5-phenylhydantoin is used as the internal standard in determining carbamazepine in whole blood or plasma. Carbamazepine is well separated from normal blood constituents in less than 8 min, and other commonly used anticonvulsants do not interfere with the analysis. The sensitivity of this method is adequate to quantitate 0.25 mg of carbamazepine per liter in 2 ml of sample, and the lower limit of detection is 100 ng. Twenty specimens were analyzed by a gas-chromatographic method and by the present method; the resulting correlation coefficient was greater than .980.

Gas Chromatographic Determination of Micro Amounts of Cyanide Residues in Wines, Distilled Liquors, and Other Alcoholic Beverages

1976 ◽  
Vol 59 (6) ◽  
pp. 1390-1395 ◽  
Author(s):  
Brian L Bates ◽  
Donald R Buick
Keyword(s):  
Cyanogen Bromide ◽  
Chromatographic Method ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Alcoholic Beverages ◽  
Relative Standard ◽  
Standard Deviations ◽  
Absorber Solution ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method for the determination of cyanide residues in alcoholic beverages has been developed from procedures previously reported for application to water samples. Quantitatively isolating HCN from alcoholic beverages presented difficulties not encountered with aqueous solutions, particularly in the presence of SO2 in the sample. HCN was liberated from the acidified sample by heating at 70°C, flushed into an NaOH absorber solution, converted to cyanogen bromide (CNBr), extracted into diisopropyl ether, chromatographed on a Porapak Q column, and detected by an electron capture detector. SO2 that is present in most wines interfered with the bromination step and caused low recoveries. This interference was eliminated by initially converting any cyanide present in the sample to the stable mercuric cyanide salt and then purging the acidified sample solution of all SO2. The Hg(CN)2 present was then dissociated by adding KI and the analysis proceeded as previously described. Mean recoveries of 80–97 % were obtained for 2–20 μg cyanide from replicate analyses of spiked samples of distilled liquors free of SO2. The relative standard deviations ranged from 6.1 to 11.1%. Mean recoveries of 65 to 91% were obtained in the same range of cyanide from replicate analyses of spiked wine samples known to contain SO2, with relative standard deviations ranging from 0.8 to 10.2%. The limit of detection was 0.2 μg HCN.

scholarly journals Quantitative determination and validation of ethylhexylglycerin using Gas chromatography method

2018 ◽  
Vol 9 (1) ◽  
pp. 30
Author(s):  
Rambabu Arla ◽  
Srinivasa Rao J ◽  
Kailasam Koumaravelou
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Stability Studies ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Ich Guidelines ◽  
Clear Peak ◽  
Gas Chromatographic Method

Ethylhexylglycerin, an alkyl glyceryl ether, used in various cosmetics and deodorants is also known to have anti-microbial activity and hence used as an adjuvant along with other preservatives to produce synergistic effect. In the present study, a gas chromatographic method has been employed and validated to determine the presence of impurities along with ethylhexylglycerin. A column having the dimension of DB-1 30m x 0.32mm; 0.25µm with acetone as solvent was found to be optimal for the ideal separation of ethylhexylglycerin from its impurities. Injection volume was set to 1 µl and temperature was maintained at 240°C. A clear peak was observed with the retention time of 8.002 minutes. As per ICH guidelines, the developed method was validated with respect to specificity, sensitivity, Limit of detection, Limit of quantification, linearity, precision, and also stability studies. As per the method, it shows a good correlation co-efficient (R2) value of 0.999 within the concentration range of 0.1- 0.75µg. Therefore, a gas chromatographic method was proposed which can be precise, specific and can be employed for the determination of ethylhexylglycerin in various pharmaceutical formulations. Keywords: Ethylhexylglycerin; Adjuvant; ICH guidelines; Validation; Stability studies

Simultaneous measurement of phenobarbital, diphenylhydantoin, and primidone in blood by high-pressure liquid chromatography.

1976 ◽  
Vol 22 (6) ◽  
pp. 824-827 ◽  
Author(s):  
P M Kabra ◽  
G Gotelli ◽  
R Stanfill ◽  
L J Marton
Keyword(s):  
High Pressure ◽  
Whole Blood ◽  
Chromatographic Method ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Blood Constituents ◽  
Liquid Chromatographic Method ◽  
Gas Chromatographic Method ◽  
Liquid Chromatographic

Abstract We describe a sensitive, precise high-pressure liquid chromatographic method in which 5-(p-methylphenyl)-5-phenylhydantoin is used as the internal standard for simultaneous determination of diphenylhydantoin, phenobarbital, and primidone in whole blood and plasma. These anticonvulsant drugs are well separated from each other and from normal blood constituents in less than 10 min. The lower limit of detection for each drug is 100 ng for primidone, 200 ng for dilantin, and 300 ng for phenobarbital. The eluted drugs were detected by their absorption at 254 nm, and evaluated from their peak heights as compared to internal standard. The method was successfully adapted for pediatric samples (100 to 500 mul of whole blood or plasma). Fifty specimens were analyzed for phenobarbital and diphenylhydantoin and 25 specimens for primidone by a standard gas-chromatographic method and by our liquid-chromatographic method; the resulting correlation coefficient was greater than 0.98.

scholarly journals Development and Validation of a Reversed-Phase High-Performance Liquid Chromatographic Method for the Simultaneous Determination of Amiloride Hydrochloride, Atenolol, Hydrochlorothiazide, and Chlorthalidone in Their Combined Mixtures

2009 ◽  
Vol 92 (2) ◽  
pp. 404-409 ◽  
Author(s):  
Abdalla A Elshanawane ◽  
Samia M Mostafa ◽  
Mohamed S Elgawish
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Chromatographic Method ◽  
High Performance Liquid Chromatographic ◽  
Ternary Mixtures ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatographic ◽  
Amiloride Hydrochloride

Abstract A high-performance liquid chromatographic method was developed for the simultaneous determination of 2 ternary mixtures containing amiloride hydrochloride, atenolol, hydrochlorothiazide, and chlorthalidone used in hypertension therapy. The use of cyanopropyl column results in satisfactory separation of both mixtures. The mobile phase consisted of 10 mM KH2PO4 buffer (pH 4.5) and methanol in a ratio of (75 25 v/v), at a flow rate of 1 mL/min. UV detector was operated at 275 nm. Calibration graphs were linear in the concentration ranges of 210, 20200, 10100, and 550 g/mL for amiloride hydrochloride, atenolol, hydrochlorothiazide, and chlorthalidone, respectively. Intraday and interday precision values (relative standard deviation) were <1.13 for mixture I (amiloride hydrochloride, atenolol, chlorthalidone), and <0.93 for mixture II (amiloride hydrochloride, atenolol, hydrochlorothiazide). The method was successfully applied for the determination of the 2 combinations in laboratory-prepared mixtures and commercial pharmaceutical formulation with high accuracy and precision. Statistical comparison of the results with those of the published methods showed excellent agreement and indicates no significant difference between them.

scholarly journals Gas Chromatographic Determination of Butylated Hydroxyanisole (BHA) and Butylated Hydroxytoluene (BHT) in Products Containing Capsaicinoids

1996 ◽  
Vol 79 (6) ◽  
pp. 1459-1462
Author(s):  
Bernard DeWitt ◽  
Gunnar Finne
Keyword(s):  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Butylated Hydroxytoluene ◽  
Butylated Hydroxyanisole ◽  
Liquid Chromatographic Method ◽  
Gas Chromatographic Method ◽  
Liquid Chromatographic

Abstract Because of interference by coeluting capsaicinoids, the commonly used liquid chromatographic method for determining butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) in pepperoni and spice blends is not reliable. A gas chromatographic method is described that cleanly separates these antioxidants from interfering substances. Average recoveries of BHA and BHT from oleoresin spiked at 5 concentrations were 97.6 and 104.3%, respectively. From pepperoni spiked at 4 levels, average recoveries were 79.1 and 87.9%, respectively. The repeatability of the method when applied to 5 replicates of pepperoni toppings was 36.4 ± 1.1 ppm for BHA and 32.2 ± 0.8 ppm for BHT.

Gas-Liquid Chromatographic Determination of T-2 Toxin in Plasma

1983 ◽  
Vol 66 (4) ◽  
pp. 909-912 ◽  
Author(s):  
Steven P Swanson ◽  
Venkatachalam Ramaswamy ◽  
Val R Beasley ◽  
William B Buck ◽  
Harold H Burmeister
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Aqueous Sodium Hydroxide ◽  
Chromatographic Determination ◽  
Florisil Column ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract The gas-liquid chromatographic method for the determination of T-2 toxin in plasma is described. The toxin is extracted with benzene, washed with aqueous sodium hydroxide, and chromatographed on a small Florisil column; the heptafluorobutyryl derivative is prepared by reaction with heptafluorobutyrylimidazole. The T-2 HFB derivative is chromatographed onOV-1 at 230°C and measured with an electron capture detector. Iso-T-2, an isomer of T-2 toxin, is added to samples as an internal standard before extraction. Recoveries averaged 98.0 ± 5.5% at levels ranging from 50 to 1000 ng/m L. The limit of detection is 25 ng/mL.

Gas-chromatographic determination of 5-fluorocytosine in human serum.

1976 ◽  
Vol 22 (6) ◽  
pp. 772-776 ◽  
Author(s):  
S A Harding ◽  
G F Johnson ◽  
H M Solomon
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Mean Value ◽  
Normal Serum ◽  
Trimethylsilyl Derivative ◽  
Serum Samples ◽  
Gas Chromatographic Method

Abstract We describe a sensitive and precise gas-chromatographic method, in which cytosine is used as the internal standard, for determination of an antifungal agent, 5-fluorocytosine, in serum. The trimethylsilyl derivative of this drug is well separated from the internal standard and from normal serum constituents. Amphotericin B does not interfere with the determination of 5-fluorocytosine. The lower limit of detection for 5-fluorocytosine is 1 mg/liter when 200 mul of serum is analyzed. Within-run precision (CV), established by analysis of 10 replicates, was 4.5% at a concentration of 19.9 mg/liter. Twenty-five serum samples were analyzed for 5-fluorocytosine by a microbiological assay and by the gas-chromatographic method. Mean value observed with the bioassay was 78.5 mg/liter and with our procedure was 69.4 mg/liter. When values for our assay were regressed against values for the bioassay, slope of the least-squares line was 0.85, intercept was 2.7 mg/liter, and r was 0.93.

scholarly journals New Liquid Chromatographic Method for Determination of Rabeprazole Sodium in Coated Tablets

2004 ◽  
Vol 87 (4) ◽  
pp. 842-846 ◽  
Author(s):  
Cássia V Garcia ◽  
Clésio S Paim ◽  
Martin Steppe
Keyword(s):  
Quantitative Determination ◽  
Proton Pump ◽  
Chromatographic Method ◽  
Array Detector ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Validation Parameters ◽  
Rabeprazole Sodium ◽  
Liquid Chromatographic

Abstract Rabeprazole sodium is a proton pump inhibitor that covalently binds and inactivates the gastric parietal cell proton pump (H+/K+ ATPase). Little has been published about the quantitative determination of this drug. The aim of this research was to develop a new liquid chromatographic method for quantitative determination of rabeprazole in coated tablets. The system consisted of a Hypersil Keystone Betabasic C8 column (250 × 4.6 mm, 5 μm particle size), an isocratic acetonitrile–water (35 + 65) mobile phase at a flow rate of 1.0 mL/min, and a diode array detector set at 282 nm. The following validation parameters were evaluated: linearity, precision, accuracy, specificity, detection and quantitation limits, and robustness. The method showed good linearity in the concentration range of 10–70 μg/mL. The quantitation limit was 2.43 μg/mL, and the detection limit was 0.80 μg/mL. The intra- and interday precision data showed that the method has good reproducibility (relative standard deviation = 1.03). Accuracy and robustness were also evaluated, and the results were satisfactory. The mean recovery was 101.61%. The analysis of a placebo mixture demonstrated the method is also specific.

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