scholarly journals Simultaneous Determination of Three Opiates in Serum by Micellar Liquid Chromatography Using Direct Injection

2005 ◽  
Vol 88 (2) ◽  
pp. 428-435 ◽  
Author(s):  
Maria-Elisa Capella-Peiró ◽  
Devasish Bose ◽  
Abhilasha Durgbanshi ◽  
Adriá Martinavarro-Domínguez ◽  
Mayte Gil-Agustí ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Direct Injection ◽  
Sodium Dodecyl ◽  
Micellar Liquid Chromatography ◽  
Optimization Criterion ◽  
Serum Samples ◽  
Intermediate Precision ◽  
Mobile Phases ◽  
Relative Standard

Abstract A simple and reliable micellar liquid chromatographic method was developed for the simultaneous determination of 3 opiates (codeine, morphine, and thebaine) in serum, using direct injection and ultraviolet detection. The separation of the drugs was optimized on a C18 column, thermostatically controlled at 25°C, by evaluating mobile phases containing sodium dodecyl sulfate (SDS) and various modifiers (propanol, butanol, or pentanol). Adequate resolution of the opiates was obtained with a chemometrics approach, in which retention was modeled as a first step by using the retention factors for several mobile phases. Next, an optimization criterion that takes into account the position and shape of the chromatographic peaks was applied. The 3 opiates were totally resolved and determined in 12 min with the mobile phase 0.15M SDS–7% (v/v) butanol buffered at pH 7. The limits of detection for codeine and morphine were greatly improved by using fluorimetric detection. Repeatability and intermediate precision were tested for 3 different concentrations of the drugs, and the relative standard deviations were <0.8% for most of the assays. Finally, the method was successfully applied to the determination of morphine and codeine in serum samples.

scholarly journals Therapeutic Drug Monitoring of Anticonvulsant Drugs by Micellar HPLC with Direct Injection of Serum Samples

2002 ◽  
Vol 48 (10) ◽  
pp. 1696-1702 ◽  
Author(s):  
Adrián Martinavarro-Domínguez ◽  
Maria-Elisa Capella-Peiró ◽  
Mayte Gil-Agustí ◽  
José V Marcos-Tomás ◽  
Josep Esteve-Romero
Keyword(s):  
Mobile Phase ◽  
Direct Injection ◽  
Sodium Dodecyl ◽  
Chromatographic Determination ◽  
Therapeutic Drug ◽  
Organic Modifiers ◽  
Serum Samples ◽  
Drug Concentrations ◽  
Mobile Phases

Abstract Background: We developed a micellar liquid chromatographic (MLC) procedure for the determination of three extensively monitored antiepileptics in serum samples: carbamazepine, phenobarbital, and phenytoin. Methods: We determined the composition of the mobile phase after modeling the elution behavior of the antiepileptics in hybrid micellar mobile phases of sodium dodecyl sulfate (SDS) with different organic modifiers (propanol, butanol, or pentanol) in an experimental design that used five mobile phases, a C18 column, and ultraviolet detection. In the micellar chromatographic system, the serum samples can be injected directly. Results: The optimum mobile phase was 70 mL/L butanol in 0.05 mol/L SDS, pH 7, in which the three antiepileptics were resolved in <10 min. Intra- and interday precision was evaluated at four different drug concentrations within the therapeutic range (n =10); CVs were <2.1%. The method was applied to the analysis of 120 serum samples, and results were similar to those obtained by the TDx® method. Conclusions: The MLC method allows chromatographic determination of three antiepileptics, using an interpretative strategy of optimization, without pretreatment of the serum samples and with direct injection in a hybrid micellar mobile phase of SDS–butanol. The method provides complete resolution and quantification of mixtures of two and three antiepileptics.

scholarly journals Micellar Liquid Chromatography for the Determination of Some Less Prescribed Benzodiazepines

2012 ◽  
Vol 9 (1) ◽  
pp. 443-450 ◽  
Author(s):  
Hoonka Subhra ◽  
Bose Devasish ◽  
Esteve-Romero Josep ◽  
Durgbanshi Abhilasha
Keyword(s):  
Analytical Chemistry ◽  
Mobile Phase ◽  
Partition Coefficients ◽  
Sodium Dodecyl ◽  
Micellar Liquid Chromatography ◽  
Serum Samples ◽  
Intermediate Precision ◽  
Chromatographic Procedure ◽  
Made In

A simple chromatographic procedure is reported for the determination of some less prescribed but equally important benzodiazepines (Clotiazepam, clozapine and pinazepam) in serum. The optimization studies have been made in CN, C18and C8columns, using mobile phase containing sodium dodecyl sulphate (SDS) modified with either propanol, butanol or pentanol. The method proposed for the determination of the three benzodiazepines using a mobile phase of 0.13 M SDS, 2.4% pentanol-0.01 M phosphate buffer- 0.1% triethylamine (pH 7) at 25°C and UV detection (240 nm) in a C8column. The serum samples was injected directly, without any pretreatment, eluted in less than 8 min, in accordance to their relative polarities, as indicated by their octanol-water partition coefficients. The limits of detection (ng/mL) was in the 1.6 to 5.6 and 7 to 87 range, for aqueous and serum samples, respectively. Repeatability and intermediate precision was tested for three different concentrations of the drugs, resulting in the 0.1 to 2 range. The results obtained here for the separation of the three benzodiazepines in serum were also counter checked at Department of Bio-analytical Chemistry, Universitat Jaume I, Castelló, Spain.

scholarly journals Monitoring Disopyramide, Lidocaine, and Quinidine by Micellar Liquid Chromatography

2011 ◽  
Vol 94 (2) ◽  
pp. 537-542 ◽  
Author(s):  
Enrique Ochoa-Aranda ◽  
Josep Esteve-Romero ◽  
Maria Rambla-Alegre ◽  
Adri Martinavarro-Domnguez ◽  
Jos V Marcos-Toms ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Direct Injection ◽  
Sodium Dodecyl ◽  
Reference Method ◽  
Micellar Liquid Chromatography ◽  
Good Resolution ◽  
Serum Samples ◽  
Spanish Hospital ◽  
Separation Temperature

Abstract A micellar liquid chromatography (MLC) method using a C18 column was developed to determine three antiarrhythmic drugsdisopyramide, lidocaine, and quinidinethat are most usually monitored in serum samples. After the application of an interpretative strategy for optimization of sodium dodecyl sulfate (SDS) and modifier concentrations in order to ensure the minimum analysis time, maximum sensitivity, and good resolution, the optimum chromatographic conditions for the determination of the three antiarrhythmics were flow rate, 1 mL/min; injection volume, 20 L; separation temperature, 25C; mobile phase, 150 mmol/L SDS-7 (v/v) butanolphosphate buffer, 10 mmol/L, pH 70.9 (w/v) NaCl; and detection at 214 nm. The calibration curves for the drugs were linear (r2 > 0.999). The intraday and interday precisions were lower than 3.9 (CV). Recoveries were 100 0.6 when the method was applied to both serum samples spiked with the antiarrhythmics (n 10) and real serum samples. In all cases, the results were similar to those obtained using the reference method (fluorescence polarization immunoassay) usually used in the Spanish hospital. The proposed method is useful for hospital monitoring of the antiarrhythmics by direct injection into the chromatograph.

Simultaneous Determination of Psychoactive Compounds in Foodstuffs Using Micellar Liquid Chromatography with Direct Injection

2014 ◽  
Vol 97 (2) ◽  
pp. 409-414 ◽  
Author(s):  
Hoonka Subhra ◽  
Dubey-Neeti Prakash ◽  
Durgbanshi Abhilasha ◽  
Esteve-Romero Josep ◽  
Bose Devasish
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Soft Drink ◽  
Direct Injection ◽  
Sodium Dodecyl ◽  
Reversed Phase ◽  
Food Samples ◽  
Micellar Liquid Chromatography ◽  
Liquid Chromatographic

Abstract A micellar liquid chromatographic procedure was developed for the simultaneous determination of threecommonly used stupefacients, lidocaine, ketamine and diazepam, using a C18 reversed-phase column. A micellar mobile phase 0.15 M sodium dodecyl sulfate and 6% (v/v) pentanol, pH 7, and UV detection at 230 nm were used to determine the three stupefacients in food samples. Using the selected mobile phase, the stupefacients were eluted in less than 10 min with linearity (r = 0.998), LOD (range: 0.004–0.03 ppm), LOQ (range: 0.004–0.03 ppm), intraday and interday precision (below 2.84%), and mean recoveries (range: 79.11–110.16%) in the different foodstuffs were in accordance with the internationally established acceptance criteria. Validation of the developed method was performed on the basis of International Conference on Harmonization validation guidelines. The optimized and validated micellar liquid chromatographic method was successfully applied in the determination of lidocaine, diazepam, and ketaminein a real food sample (mango drink) and in spiked food samples (banana, ladoo, soft drink, tea). The developed method could also be easily used by law enforcement laboratories and hospitals for routine analysis.

scholarly journals Determination of Disulfiram by Micellar Liquid Chromatography in Illicit Preparations

2011 ◽  
Vol 94 (4) ◽  
pp. 1082-1088 ◽  
Author(s):  
Sandeep-Kumar mourya ◽  
Swati Dubey ◽  
Abhilasha Durgabanshi ◽  
Sudheer Kumar Shukla ◽  
Josep Esteve-Romero ◽  
...  
Keyword(s):  
Direct Injection ◽  
Sodium Dodecyl ◽  
Micellar Liquid Chromatography ◽  
Blood Levels ◽  
Pharmacokinetic Studies ◽  
Optimization Strategy ◽  
Recovering Alcoholics ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic

Abstract Presently, disulfram is used in aversion therapy for recovering alcoholics. It acts by inhibiting aldehyde dehydrogenase, leading to high blood levels of acetaldehyde. A simple direct injection micellar liquid chromatographic procedure was developed to determine disulfram in illicit preparations (ayurvedic, herbal, divine ash, and traditional medicine), as well as inpharmaceuticals and biological samples (urine). After application of a predictive optimization strategy, the proposed method was developed using a 0.1 M sodium dodecyl sulfate-butanol 4% (v/v) buffered to pH 7 as the mobile phase at a flow rate of 1 mL/min, an octyl silyl (C8) 150 mm column, and diode array detection at 248 nm. Under the above conditions, the analysis time was below 8 min. Validation studies were based on U.S. Food and Drug Administration guidelines. The LOD (3 × SD criterion) was 15 ng/mL and LOQ (10 × SD criterion) was 70 ng/mL for disulfram. The intraday and interday precisions were below 3.5%, recoveries were in the range of 97–102%, and robustness was below 3%. The optimized and validated micellar liquid chromatographic method was successfully applied to the determination of disulfram in ayurvedic, herbal, divine ash, and other samples. The procedure developed could also be used in the felds of QC, routine analysis, and pharmacokinetic studies.

A Rapid and Sensitive HPLC-FLD Method for the Determination of Retinol and Vitamin E Isomers in Human Serum

2019 ◽  
Vol 15 (7) ◽  
pp. 745-752
Author(s):  
Yi Yang ◽  
Dan Lu ◽  
Danni Yang ◽  
Shuo Yin ◽  
Jing Zhang ◽  
...  
Keyword(s):  
Vitamin E ◽  
Human Serum ◽  
Simultaneous Determination ◽  
Fluorescence Detection ◽  
High Performance ◽  
Correlation Coefficients ◽  
Serum Samples ◽  
Rapid Separation ◽  
Relative Standard

Background: Retinol and vitamin E are fat-soluble vitamins crucial for human health, yet their isomers’ distributions in the human body are still known roughly. In order to figure out the physical condition and evaluate the nutritional status of an individual, it is imperative to analyze retinol and VE isomers in human serum. Objective: This work aims to establish a rapid and simple high-performance liquid chromatography with fluorescence detection for simultaneous determination of retinol and vitamin E isomers in human serum. Methods: Separation was accomplished on a common C18 column thermostated at 25 oC, using a simple isocratic elution program of methanol/acetonitrile (85:15, v/v) at a flow rate of 1.0 mL/min. Fluorescence detection was operated using excitation/emission wavelengths of 329 nm/472 nm for retinol and 294 nm/338 nm for VE isomers, respectively. Results: Rapid separation was achieved within 13 min. Linear ranges of the method were 0.020-50.0 µg/mL, with correlation coefficients greater than 0.999. Detection limits and the quantification limits were 0.001-0.004 µg/mL and 0.003- 0.013 µg/mL, respectively. Mean recoveries were 84.1%- 98.2%, with intra-day and inter-day relative standard deviations less than 12.3% and 13.6%, respectively. This method has been applied to the simultaneous determination of retinol and 8 VE isomers in human serum samples with satisfactory results. Conclusion: A rapid, simple and robust method was developed for routine analysis of retinol and eight vitamin E isomers in human serum, providing a useful tool for clinical diagnosis and nutritional evaluation.

Simultaneous Determination of Cationic and Anionic Surfactants in Domestic, Sewage and River Effluent by Diffuse Reflectance -Fourier Transform Infrared Spectroscop ic Analysis

2021 ◽  
Vol 30 (1) ◽  
pp. 32-40 ◽  
Author(s):  
Ramsingh Kurrey ◽  
Kaushlya Thakur ◽  
Swati Chandrawanshi ◽  
Manas Kanti Deb
Keyword(s):  
Fourier Transform ◽  
Standard Deviation ◽  
Simultaneous Determination ◽  
Diffuse Reflectance ◽  
Limit Of Detection ◽  
Sodium Dodecyl ◽  
Fourier Transform Infrared ◽  
Domestic Sewage ◽  
Relative Standard

A new, simple, rapid and precise novel hyphenated diffuse reflectance-Fourier transform infrared spectroscopy (DRS-FTIR) technique for the simultaneous determination of the most frequently used cationic surfactants (CS+) i.e. cetyltrimethylammonium bromide (CTAB) and anionic surfactant (AS-) i.e. sodium dodecyl sulphate (SDS) in domestic, sewage and river wastewater samples has been stabilised. CS+ and AS- were analyzed using DRS-FTIR, the most steady and strongest vibrational IR peak at 2917.13 cm-1 for CTAB and 1226.07 for SDS were selected for the simultaneous quantiflcation of CS+ and AS- under the optimized condition such as effect of samples volume and effect of temperature. The limit of detection (LOD) and limit of quantiflcation (LOQ) of the present method were 5 µg/mL and 15 µg/mL, respectively. The absorbance and peak area were determined by the DRS-FTIR method, which shows excellent linearity with a correlation coefflcient value of 0.985 and 0.981 for the concentration range of 10-100 µg/mL. The standard deviation (SD) and relative standard deviation (RSD) for six replicate measurements were found to be 0.052 µg/L and 2.8 %, respectively.

scholarly journals Development of Micellar HPLC-UV Method for Determination of Pharmaceuticals in Water Samples

2018 ◽  
Vol 2018 ◽  
pp. 1-12 ◽  
Author(s):  
Danielle Cristina da Silva ◽  
Cláudio Celestino Oliveira
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Solid Phase ◽  
Sodium Dodecyl ◽  
Micellar Liquid Chromatography ◽  
Phase Extraction ◽  
Mobile Phases ◽  
Concentration Factors ◽  
Better Than

Method for extraction and determination of amoxicillin, caffeine, ciprofloxacin, norfloxacin, tetracycline, diclofenac, ibuprofen, nimesulide, levonorgestrel, and 17α-ethynylestradiol exploiting micellar liquid chromatography with PDA detector and solid-phase extraction was proposed. The usage of toxic solvents was low; the chromatographic separation of the medicaments was performed using a C18 column and mobile phases A and B containing 15.0% (v/v) ethanol, 3.0% (m/v) sodium dodecyl sulfate (SDS), and 0.02 mol·L−1 phosphate at pHs 7.0 and 8.0, respectively. The method is simple, selective, and fast, and the analytes were separated in 23.0 min. For extraction, 1000 mL of sample containing 2.0% (v/v) ethanol and 0.002 mol·L−1 citric acid at pH 2.50 was loaded through a 1000 mg of C18 cartridge. The analytes were eluted using 3.0 mL of ethanol, which were evaporated and redissolved in 0.5 mL of mobile phase. Concentration factors better than 1200, except amoxicillin (224), were obtained. The analytical curves were linear (R2 better than 0.992); LOD and LOQ n=10 presented values in the range of 0.019–0.247 and 0.058–0.752 mg·L−1, respectively. Recoveries of 99% were obtained, and the results are in agreement with those obtained by the comparative methods.

scholarly journals UHPLC-PDA Assay for Simultaneous Determination of Vitamin D3and Menaquinone-7 in Pharmaceutical Solid Dosage Formulation

2017 ◽  
Vol 2017 ◽  
pp. 1-9 ◽  
Author(s):  
Muhammad Jehangir ◽  
Mahmood Ahmed ◽  
Muhammad Imtiaz Shafiq ◽  
Abdul Samad ◽  
Iftikhar-ul-Haq
Keyword(s):  
Vitamin D ◽  
Simultaneous Determination ◽  
Hplc Method ◽  
Coefficient Of Determination ◽  
Solid Dosage ◽  
Mobile Phases ◽  
Relative Standard ◽  
Repeatability And Reproducibility ◽  
Ultrahigh Performance Liquid Chromatography

A newly developed method based on ultrahigh performance liquid chromatography (UHPLC) was optimized for the simultaneous determination of vitamin D3and menaquinone-7 (MK-7) in tablet formulation in the present study. UHPLC separation of vitamin D3and MK-7 was performed with ACE Excel 2 C18-PFP column (2 μm, 2.1×100 mm) at 0.6 mL min−1flow rate, whereas the mobile phase consisted of methanol/water (19:1, v/v, phase A) and isopropyl alcohol (99.9%, phase B) containing 0.5% triethylamine. Isocratic separation of both the analytes was performed at 40°C by pumping the mobile phases A and B in the ratio of50:50(v/v, pH, 6.0). Both analytes were detected at a wavelength of 265 nm and the injection volume was 1.0 μL. The overall runtime per sample was 4.5 min with retention time of 1.26 and 3.64 min for vitamin D3and MK-7, respectively. The calibration curve was linear from 5.0 to 100 μg mL−1for vitamin D3and MK-7 with a coefficient of determination (R2)≥0.9981, while repeatability and reproducibility (expressed as relative standard deviation) were lower than 1.46 and 2.21%, respectively. The proposed HPLC method was demonstrated to be simple and rapid for the determination of vitamin D3and MK-7 in tablets.

scholarly journals Development and validation of an LC-MS/MS method for the determination of adapalene in pharmaceutical forms for skin application

2016 ◽  
Vol 81 (10) ◽  
pp. 1171-1181 ◽  
Author(s):  
Vladimir Dobricic ◽  
Natasa Bubic-Pajic ◽  
Bojan Markovic ◽  
Sote Vladimirov ◽  
Snezana Savic ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Ammonium Acetate ◽  
Intermediate Precision ◽  
Column Temperature ◽  
Mobile Phases ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Chromatographic Parameters ◽  
Development And Validation

Development and validation of a liquid chromatography - tandem mass spectrometry (LC-MS/MS) method for the determination of adapalene in pharmaceutical forms for skin application were presented. The MS/MS analysis of adapalene was performed by use of three mobile phases, consisted of acetonitrile and (a) 0.1 % formic acid, (b) 0.1 % trifluoroacetic acid and (c) 20 mM ammonium acetate. The strongest signals of parent ion and dominant product ion were obtained in negative mode by use of the mobile phase (c). Validation of this method was performed according to the ICH guidelines. Small variations of selected chromatographic parameters (concentration of ammonium acetate, mobile phase composition, column temperature and flow rate) did not affect qualitative and quantitative system responses significantly, which proved method?s robustness. The method is specific for the determination of adapalene. Linearity was proved in the concentration range 6.7 - 700.0 ng mL-1 (r = 0.9990), with limits of detection and quantification 2.0 ng mL-1 and 6.7 ng mL-1, respectively. Accuracy was confirmed by calculated recoveries (98.4 % - 101.5 %). Precision was tested at three levels: injection repeatability, analysis repeatability and intermediate precision. Calculated relative standard deviations were less than 1, 2 and 3 %, respectively.

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