Dual design spaces for micro-extraction together with the core–shell chromatographic determination of dorzolamide and timolol in rabbit plasma: an example of quality by design method development

2016 ◽  
Vol 40 (10) ◽  
pp. 8424-8437 ◽  
Author(s):  
Abdel-Maaboud Ismail Mohamed ◽  
Hanaa Mohammed Abdel-Wadood ◽  
Heba Salah Mousa

An innovative quality by design-integrated VA-SALLME-core–shell chromatographic method was developed for the simultaneous determination of DOR and TIM in plasma.

Author(s):  
Budideti Kishore Kumar Reddy ◽  
Kothapalli Bonnoth Chandra Sekhar ◽  
Chinnala Krishna Mohan

A simple, reproducible bioanalytical method of liquid chromatography and PDA detector was developed and validated for the simultaneous Determination of Vildagliptin and Telmisartan in Rabbit Plasma using liquid-liquid extraction technique. K2 EDTA was used as anti-coagulant. Analytes were extracted by Methyl-tert-Butyl Ether (MTBE) and subsequent separation on a Kromasil C18 column (5 µ, 100 × 4.6 mm) using Acetonitrile : Methanol 75:25 v/v as mobile phase at a flow rate of 1 mL/min and (40±1)°C column oven temperature. Analytes were monitored with PDA detector at an isosbestic point of 225 nm for both Vildagliptin and Telmisartan.  Retention times of Vildagliptin and Telmisartan were found to be at 2.545 mins and 6.633 mins respectively. The method was validated over a linear (r2 = 0.9979) concentration range of 24.979 - 5003.808  µg/ml for Vildagliptin and 1.011- 202.559 µg/ml for Telmisartan. The inter-day and intra-day precisions were found to be less than 15% and the accuracy was all within ±15% (at LLOQ ±20%). The developed HPLC-PDA method was fully validated for all the other parameters as per FDA guidelines like selectivity, matrix effect, recovery and stability as well. Due to the high degree of sensitivity, very less time consuming, easy extraction procedure and low requirement of sample volume, the method will be applicable for therapeutic drug monitoring.


1968 ◽  
Vol 51 (1) ◽  
pp. 24-28
Author(s):  
George Yip ◽  
Samuel F Howard

Abstract A gas chromatographic method for the simultaneous determination of four dinitrophenolic herbicides [dinitrocresol (DNOC), dinitrobutylphenol (DNBP), dinitroamylphenol (DNAP), and dinitrocyclohexylphenol (DNOCHP)] in crops has been developed. After a 50 g sample was extracted with chloroform, a 10 g aliquot was concentrated and reacted with diazomethane to form the methyl ether derivatives. The sample was subjected to a two column cleanup step. acid-Celite and Florisil, and the residue was analyzed by GLC with an electron capture detector. Recoveries of fortification levels of 0.1 ppm DNOC and 0.2 ppm DNBP, DNAP, and DNOCHP exceeded 80%. The crops studied included green beans, pole beans, lima beans, peas, apples, and oranges.


2012 ◽  
Vol 2 (2) ◽  
pp. 364-367 ◽  
Author(s):  
Saida Naik Dheeravath ◽  
◽  
Kasani Ramadevi ◽  
Zilla Saraswathi ◽  
Dheeravath Maniklal ◽  
...  

2019 ◽  
Vol 15 (6) ◽  
pp. 635-641
Author(s):  
Nadia M. Mostafa ◽  
Ghada M. Elsayed ◽  
Nagiba Y. Hassan ◽  
Dina A. El Mously

Background:The concept of green analytical chemistry prevails due to the growing environmental pollution.Objective:Our attempts are to develop simple and eco-friendly method which is non-harmful to the environment by producing minimal waste. In this context, a green liquid chromatographic method was applied for the simultaneous determination of chlorpheniramine maleate, pseudoephedrine hydrochloride and propyphenazone in their combined dosage form.Methods:Separation was carried out using X select HSS RP C18 analytical column (250 × 4.6 mm, 5μm) using methanol - 0.02 M phosphate buffer pH 3 - triethylamine (60:40: 0.1, by volume) as a mobile phase. The separated peaks were detected at 215 nm at a flow rate 1.0 mL/min.Results:Quantification was done over the concentration ranges of 1-25 µg/mL for chlorpheniramine maleate, 5-35 µg/mL for pseudoephedrine hydrochloride and 10-120 µg/mL for propyphenazone. The suggested method was validated with regard to linearity, accuracy and precision according to the International Conference on Harmonization guidelines with good results.Conclusion:It could be used as a safer alternative for routine analysis of the mentioned drugs in quality control laboratories.


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