Application of a liquid chromatographic procedure for the analysis of penicillin antibiotics in biological fluids and pharmaceutical formulations using sodium dodecyl sulphate/propanol mobile phases and direct injection

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.

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Direct Injection Microemulsion HPLC Method for Simultaneous Determination of Morphine, Tramadol and Lornoxicam in Biological Fluids Using Monolithic Column

Current Pharmaceutical Analysis ◽

10.2174/1573412915666190617172144 ◽

2020 ◽

Vol 16 (8) ◽

pp. 1148-1156

Author(s):

Fathalla Belal ◽

Mahmoud A. Omar ◽

Sayed M. Derayea ◽

Sahar Zayed ◽

Mohamed A. Hammad ◽

...

Keyword(s):

Orthophosphoric Acid ◽

Biological Fluids ◽

Monolithic Column ◽

Direct Injection ◽

Sodium Dodecyl ◽

Hplc Method ◽

Mobile Phase Flow Rate ◽

Plasma And Urine Samples ◽

Detection Mode ◽

Liquid Chromatographic

Objective: A rapid and environmental friendly microemulsion liquid chromatographic method was developed for simultaneous quantification of morphine (MOR), tramadol (TRA) and lornoxicam (LOR) in biological fluids. Methods: Microemulsion used in this study was an aqueous solution containing sodium dodecyl sulfate (0.12 M), n-propanol (10%), ethyl acetate (0.75%), tri-ethyl amine (0.3%), orthophosphoric acid (0.15 %) and the pH was adjusted to 3.0 with orthophosphoric acid. Chromatographic separation was carried out on a monolithic C18 column and a mobile phase flow rate of 1.0 mL min−1 was applied throughout the analysis. The data was monitored using UV-detection mode at a wavelength of 220 nm. Results: Under the optimized conditions, all the studied drugs were well resolved and completely eluted within 6 min. The proposed method was linear over the concentration ranges of 0.5−100, 0.75−125 and 0.25−50 μg mL−1; limits of detection of 0.074, 0.086 and 0.056 μgmL−1 and limits of quantification of 0.21, 0.28 and 0.12 were recorded for TRA, LOR, and MOR, respectively. The developed method was fully validated according to the ICH guidelines. The method was successfully utilized to estimate the tested analytes in plasma and urine samples, which were directly injected into the chromatographic system after suitable dilution with the microemulsion. Conclusion: The developed method is considered to be very efficient to analyze the cited drugs in different biological fluids with low running costs and short analysis time.

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Spectrofluorometric Determination of Verapamil Hydrochloride in Pharmaceutical Preparations and Human Plasma Using Organized Media: Application to Stability Studies

Journal of AOAC International ◽

10.1093/jaoac/89.6.1565 ◽

2006 ◽

Vol 89 (6) ◽

pp. 1565-1572 ◽

Cited By ~ 7

Author(s):

Mohamed Walash ◽

Fathalla Belal ◽

Nahed El-Enany ◽

Amina Abdelsalam

Keyword(s):

Human Plasma ◽

Biological Fluids ◽

Sodium Dodecyl ◽

Pharmaceutical Preparations ◽

Pharmaceutical Formulations ◽

Official Method ◽

Stability Studies ◽

Verapamil Hydrochloride ◽

Spiked Human Plasma

Abstract A highly sensitive spectrofluorometric method was developed for the determination of verapamil hydrochloride (VP HCl) in pharmaceutical formulations and biological fluids. The proposed method is based on investigation of the fluorescence spectral behavior of VP HCl in micellar systems, such as sodium dodecyl sulfate (SDS) and β-cyclodextrin (β-CD). In aqueous solutions of borate buffer of pH 9 and 8.5, VP HCl was well incorporated into SDS and β-CD, respectively, with enhancement of its native fluorescence. The fluorescence was measured at 318 nm after excitation at 231 nm. The fluorescence intensity enhancements were 183 and 107% in SDS and in β-CD, respectively. The fluorescence-concentration plots were rectilinear over the range of 0.020.2 and 0.020.25 μg/mL, with lower detection limits of 5.58 × 103 and 3.62 × 103 μg/mL in SDS and β-CD, respectively. The method was successfully applied to the analysis of commercial tablets and the results were in good agreement with those obtained with the official method. The method was further applied to the determination of VP HCl in real and spiked human plasma. The mean % recoveries in the case of spiked human plasma (n 4) was 92.59 3.11 and 88.35 2.55 using SDS and β-CD, respectively, while that in real human plasma (n 3) was 90.17 6.93 and 89.17 6.50 using SDS and β-CD, respectively. The application of the method was extended to the stability studies of VP HCl after exposureto ultraviolet radiation and upon oxidation with hydrogen peroxide.

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Comparison of surfactant-mediated liquid chromatographic modes with sodium dodecyl sulphate for the analysis of basic drugs

Analytical Methods ◽

10.1039/d0ay00526f ◽

2020 ◽

Vol 12 (19) ◽

pp. 2443-2452 ◽

Cited By ~ 2

Author(s):

N. Pankajkumar-Patel ◽

E. Peris-García ◽

M. J. Ruiz-Angel ◽

M. C. García-Alvarez-Coque

Keyword(s):

Sodium Dodecyl Sulphate ◽

Sodium Dodecyl ◽

Basic Drugs ◽

Comprehensive Overview ◽

Basic Compounds ◽

Liquid Chromatographic

A comprehensive overview of the performance of MLC, HSLC and MELC for the analysis of basic compounds.

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

International Journal of Analytical Chemistry ◽

10.1155/2012/809513 ◽

2012 ◽

Vol 2012 ◽

pp. 1-7 ◽

Cited By ~ 10

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.

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Fluorometric determination of indocyanine green in plasma.

Clinical Chemistry ◽

10.1093/clinchem/33.6.765 ◽

1987 ◽

Vol 33 (6) ◽

pp. 765-768 ◽

Cited By ~ 23

Author(s):

B Hollins ◽

B Noe ◽

J M Henderson

Keyword(s):

Indocyanine Green ◽

Limit Of Detection ◽

Degradation Products ◽

Biological Fluids ◽

Complete Analysis ◽

Spectrophotometric Methods ◽

Specificity And Sensitivity ◽

Order Of Magnitude ◽

Chromatographic Procedure ◽

Liquid Chromatographic

Abstract With this fluorometric method for measuring indocyanine green (ICG) in biological fluids, the limit of detection is an order of magnitude lower than for the traditional spectrophotometric procedure. The excitation and emission maxima are 780 and 810 nm, respectively. Agreement was excellent (r = 0.998) between direct results by this method and those by a liquid-chromatographic procedure with spectrophotometric detection. ICG breaks down in aqueous solution; the degradation products can be detected with liquid-chromatographic/spectrophotometric methods, but because the metabolites are not fluorescent, they do not interfere in the method present here. The increased specificity and sensitivity of this method should permit much more complete analysis of the kinetics of ICG disposition.

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

Clinical Chemistry ◽

10.1093/clinchem/48.10.1696 ◽

2002 ◽

Vol 48 (10) ◽

pp. 1696-1702 ◽

Cited By ~ 23

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.

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