scholarly journals Simultaneous determination of methanol, ethanol and isopropanol in human blood and white spirit samples

Author(s):  
Phuong Vu Anh ◽  
Ngan Nguyen Thi ◽  
Trang Do Thi ◽  
Luong Dinh Son ◽  
Anh Huong Nguyen Thi ◽  
...  

A simple and cost-effective method for simultaneous determination of methanol, ethanol, and isopropanol in human blood and white spirit samples using headspace gas chromatography coupled with flame ionization detection (HS-GC-FID) was developed and validated for clinical and toxicological purposes. In this study, the headspace sampling procedure was investigated, indicating optimized temperature of 70 °C in 20 min. Concentrations of target compounds were determined by internal standard (IS) method with acetonitrile as IS compound. A good resolution of chromatographic peaks was achieved. The linear ranges for all the compounds were from 1 to 500 mg/dL. Our method was validated with adequate accuracy (recovery > 98%) and precision (RSD < 0.1%) in whole human blood and white spirit samples. The limits of detection were below 0.5 mg/L for the three compounds. This method is easy to perform, making it suitable for routine analysis in clinical biochemistry and forensic laboratories.

2011 ◽  
Vol 8 (1) ◽  
pp. 391-399 ◽  
Author(s):  
Indrajit Sen ◽  
Ajay Shandil ◽  
Manjeet Aggarwal ◽  
Rakesh Kumar Khandal

A gas chromatographic method developed and validated for simultaneous determination of lindane and carbaryl for quality evaluation of lindane-carbaryl granule, using a glass capillary HP5 column (30 m x 0.32 mm; 0.25 μm), temperature programming with flame ionization detector and dibutylphthalate as an internal standard. The calibration graphs were found linear in the concentration range of 1 μg/mL to 1000 μg/mL for both lindane and carbaryl with correlation coefficient of 0.999 and 0.999 respectively and co-efficient of variation for intra-day and inter-day repeatability studies at different concentration levels was found to be less than 2%. The accuracy of method ranges between 98.5% to 100.8%. Specificity and robustness were also within the acceptable range. The method is highly sensitive with LOD and LOQ as 0.5 and 2 μg/mL for lindane and carbaryl respectively. The method has been tried on several formulations of lindane-carbaryl granules for quality control and has been found to be applicable.


Author(s):  
Siyao Jin ◽  
Qing Zhao ◽  
Dongjie Zhang ◽  
Zhigang Zhao ◽  
Shenghui Mei

AbstractLamotrigine (LTG) and oxcarbazepine (OXC) are first-line drugs for epilepsy treatment. Their large pharmacokinetics variabilities and relations between efficacy and toxicity and blood plasma concentration require routine monitoring for dose adjustment. In this study, we developed and validated a simple, accurate, and reliable method for simultaneous determination of LTG, OXC and 10,11-dihydro-10-hydroxycarbazepine (MHD) in human blood plasma by high-performance liquid chromatography-ultraviolet detection (HPLC-UV) with a simple one-step protein precipitation using methanol (1% acetic acid) and 15 min elution time under isocratic elution at 1 mL/min. Calibration range was 2.4 to 120 mg/L for LTG, OXC, and MHD. The intra-day and inter-day bias were − 8.84 to 4.18%, and the imprecision was less than 8.08% for all analytes. The internal standard (fluconazole) normalized recovery was 96.30 to 107.69% for LTG, 98.51 to 111.04% for MHD, and 95.04 to 109.86% for OXC. A total of 186 LTG samples and 25 MHD samples were used to evaluate the agreement between HPLC-UV and ultra-performance liquid chromatography-mass spectrometry (UHPLC-MS/MS) by Passing-Bablok regression and Bland-Altman plot. The mean bias and the 95% limits of agreement (95% LOA) of the two measurements were 0.575 mg/L and − 1.238 to 2.387 mg/L for LTG (n = 186) and − 1.222 mg/L and − 8.271 to 5.827 mg/L for MHD (n = 25), which indicated the UV method was comparable with the MS method for LTG and MHD analysis.


1983 ◽  
Vol 48 (3) ◽  
pp. 722-734
Author(s):  
Martin Koval

The flame ionisation detector response to C6-C11 aliphatic hydrocarbon solutions in carbon disulphide in the concentration range between 1.3-9.5 mg ml-1 retained lineary despite the excess of solvent entering the detector simultaneously with the analyte. Pure carbon disulphide exhibited a small positive detector response which did not interfere in calibration procedure and which, under certain GC conditions, inverted to negative values. This response was not proportional to the injected volume and was strongly influenced by the column temperature and/or bleed. On the basis of these findings, a method compatible with the widely used charcoal tube carbon disulphide desorption procedure was developed and evaluated. It consists of static desorption of the sum of aliphatic alkanes and cycloalkanes from the activated charcoal after which an internal standard is added to the supernatant eluate. The resulting carbon disulphide solution is analysed on a highly polar stationary phase 1,2,3-tris(2-cyanoethoxy)propane where the solvent and the analyte coelute in a single peak, the height of which is practically proportional to the sum of alkanes and cycloalkanes present. This also makes determinations of other substances present in the sample more simple. The field test of the proposed method yielded values comparable in precision and accuracy with a control infrared spectrophotometric method.


Author(s):  
Hina Shamshad ◽  
Ali Sayqal ◽  
Jahan Zeb ◽  
Agha Zeeshan Mirza

Abstract A simple, accurate and precise RP-HPLC method was developed for the simultaneous determination of chloroquine, pyrimethamine and cetirizine hydrochloride concentrations in bulk drug and human serum. The assay was performed using a mobile phase of methanol: water (70:30) at pH of 2.8 ± 0.05 on the Purospher C-18 column with UV detection at 230 nm and rosuvastatin used as an internal standard. The retention times observed for chloroquine, pyrimethamine and cetirizine hydrochloride were 3.5, 2.5 and 5.5 minutes, respectively. The method was found to be specific for the assayed drugs showing a linear response in the concentration range of 1–100 μg mL−1 with coefficients of determination values of (r = 0.999). The method was developed and validated according to ICH guidelines. The method was used to monitor the serum samples and was found to be sensitive for therapeutic purposes, showing the potential to be a useful tool for routine analysis in laboratories.


2017 ◽  
Vol 15 (1) ◽  
pp. 293-298
Author(s):  
Pakinaz Y. Khashaba ◽  
Hassan Refat H. Ali ◽  
Mohamed M. El-Wekil

AbstractA simple, rapid, cost-effective, and sensitive TLC-spectrodensitometric method for simultaneous determination of esomeprazole and domperidone was developed and tested in human plasma. Ethyl acetate: methanol: benzene: acetonitrile (5: 4: 8: 3, v/v/v/v) mobile phase was used for separation on TLC plates detected at 286 nm. The linearity ranges were 5-1200 and 2-600 ng/ spot for esomeprazole and domperidone, and limits of detection were 1.73 and 0.59 ng/spot. The effects of four variables affecting Rf were evaluated by fractional factorial design. The benzene volume and saturation time had significant effects.


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