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 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 Micellar Liquid Chromatographic Determination of Carbaryl and 1-Naphthol in Water, Soil, and Vegetables

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Mei-Liang Chin-Chen ◽  
Maria Rambla-Alegre ◽  
Abhilasha Durgbanshi ◽  
Devasish Bose ◽  
Sandeep K. Mourya ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Cetylpyridinium Chloride ◽  
Sodium Dodecyl ◽  
Chromatographic Determination ◽  
Limit Of Quantification ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

A liquid chromatographic procedure has been developed for the determination of carbaryl, a phenyl-N-methylcarbamate, and its main metabolite 1-naphthol, using a C18 column (250’mm’ × ’4.6’mm) with a micellar mobile phase and fluorescence detection at maximum excitation/emission wavelengths of 225/333’nm, respectively. In the optimization step, surfactants sodium dodecyl sulphate (SDS), Brij-35 andN-cetylpyridinium chloride monohydrate, and organic solvents propanol, butanol, and pentanol were considered. The selected mobile phase was 0.15’M SDS-6% (v/v)-pentanol-0.01’M NaH2PO4buffered at pH 3. Validation studies, according to the ICH Tripartite Guideline, included linearity (r>0.999), limit of detection (5 and 18’ng mL-1, for carbaryl and 1-naphthol, resp.), and limit of quantification (15 and 50’ng mL-1, for carbaryl and 1-naphthol, resp.), with intra- and interday precisions below 1%, and robustness parameters below 3%. The results show that the procedure was adequate for the routine analysis of these two compounds in water, soil, and vegetables samples.

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 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 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.

Liquid-chromatographic determination of ciprofloxacin in serum and urine.

1985 ◽  
Vol 31 (5) ◽  
pp. 684-686 ◽  
Author(s):  
D E Nix ◽  
J M De Vito ◽  
J J Schentag
Keyword(s):  
Mobile Phase ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Multiple Drug ◽  
Serum Samples ◽  
Acid Urine ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Serum And Urine

Abstract We describe the liquid-chromatographic determination of ciprofloxacin in patients' serum and urine. Serum samples were prepared by precipitating protein with perchloric acid. Urine samples were diluted 100-fold with mobile phase. The mobile phase, consisting of pH 3 phosphate buffer/acetonitrile/methanol (81/5/14, by vol), was pumped through a mu Bondapak C18 reversed-phase column at 1.5 mL/min. Fluorescence of the effluent was monitored, at wavelengths for excitation and emission of 270 and 440 nm, respectively. Standard curves were linearly related to concentration from 0.08 to 10 mg/L for serum, 1 to 20 mg/L for urine. The procedure was evaluated in a clinical setting to determine its usefulness in studying the pharmacokinetics of ciprofloxacin in patients with concurrent diseases and receiving multiple drug therapies.

The Dtermination of Paracetamol by HPLC Validation of the Method and Application on Serum Samples

2018 ◽  
Vol 69 (3) ◽  
pp. 627-631 ◽  
Author(s):  
Viorica Ohriac (Popa) ◽  
Diana Cimpoesu ◽  
Adrian Florin Spac ◽  
Paul Nedelea ◽  
Voichita Lazureanu ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Hplc Analysis ◽  
Emotional Experience ◽  
Optimum Conditions ◽  
Serum Samples ◽  
Liquid Chromatograph ◽  
Mobile Phase Flow Rate ◽  
Quantification Limit

Pain is defined as a disagreeable sensory and emotional experience related to a tissue or potential lesion. Paracetamol (Acetaminophen) is the most used non-morphine analgesic. For the determination of paracetamol we developed and validated the high performance liquid chromatography (HPLC) analysis using a Dionex Ultimate 3000 liquid chromatograph equipped with a multidimensional detector. After determining the optimum conditions of analysis (80/20 water / acetonitrile mobile phase, flow rate 1.0 mL / min, detection wavelength 245 nm) we validated the method following the following parameters: linearity of response function, linearity of results, limit (LD = 0.66 mg / mL) and quantification limit (LQ = 2.00 mg / mL), and precision. The method of determining paracetamol by HPLC was applied to 30 samples of serum collected from patients who had pain and were treated with paracetamol.

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