Mohd Idris

Simultaneous determination of methaqaulone, saccharin, paracetamol, and phenacetin in illicit drug samples by hplc

BackgroundSaccharin, a low calorie artificial sweetener was found as a new diluent / adulterant present along with paracetamol and phenacetin in an illicit methaqualone sample.MethodsAll these components were simultaneously analyzed by the proposed reverse phase high performance liquid chromatography method using C18 column using acetonitrile: water (90:10 v/v) as mobile phase with a flow rate of 1mL / min.ResultsThe percentages of saccharin, phenacetin, paracetamol and methaqualone in illicit drug sample were found to be 15.0, 45.6, 25.1 and 12.0 respectively. The method was validated for limit of detection, limit of quantification, linearity, accuracy, precision and reproducibility with the help of the exhibit and simulated samples.ConclusionsThe proposed method is simple, accurate and fast. It can be applied to the routine analysis of illicit methaqualone samples as well as for their impurity profiles for tracing the origin.

Rhodamine-Sulphuric Acid -A New Visualization Reagent for the Determination of Sucralose by HPTLC

Sucralose a UV-visible inactive compound was separated on silica gel plate without any plate treatment prior to analysis, derivatized with rhodamine - sulphuric acid reagent and detected densitometrically at 456 nm as olive green band. With this reagent sucralose also shows golden yellow fluorescence at 366 nm. Two new solvent systems i.e. chloroform: methanol: toluene (v/v 5:3.5:1.5) (solvent system-I) and chloroform: ethanol: benzene (v/v 5:3:2) (solvent system-II) were developed and giving Rf values of 0.62 and 0.45 respectively. The method was found to be sensitive with good limit of detection (LOD) for two solvent systems. The method imparts specificity to the method as at 456 nm sucralose only gives olive green color spots where as other artificial sweeteners did not show any response to this reagent, where as carbohydrates gives black color spots. Similarly sucralose gives golden yellow fluorescence at 366 nm which is not given by any other artificial sweetener. The method was highly reproducible with relative standard deviation (RSD)≤3% (n=3) and was applied for the determination of sucralose in different matrices like cola drinks, lemon juices, sugar free sweets, tabletop sweeteners etc.etc.

Determination of free duloxetine in human serum by high-performance thin-layer chromatography

A rapid, sensitive, and specific high-performance thin-layer chromatographic (HPTLC) method was developed and validated for quantitative determination of free duloxetine (DLX) in human serum. Densitometric analysis of free DLX was carried out at 235 nm after simple liquid-liquid extraction. The method uses thinlayer chromatography (TLC) aluminum plates pre-coated with silica gel G 60 F254 as stationary phase and acetone-benzene-triethylamine (5:4.5:0.5, v/v) as mobile phase for the separation of free DLX from serum constituencies. The calibration curve was linear (r2 = 0.980) in the tested range of 35–140 ng spot−1 with a limit of quantification and detection of 35 and 10 ng spot−1 with the recovery of free DLX in serum ranges from 92.86 to 97.58%. Intra- and inter-day precision (% RSD) values were ≤1.83% and ≤5.66%, respectively. Analysis of free DLX from human serum was successfully performed without interference from endogenous materials and some of the other common drugs of abuse. The method’s ability to quantify free DLX with precision, accuracy, and sensitivity makes it useful in forensic examination.

High-performance thin-layer chromatography analysis of saccharin in foods and beverages

A simple, accurate, and inexpensive high-performance thin-layer chromatography (HPTLC) method has been established for analysis of saccharin in foodstuffs, for example cola drinks, lemon juices, betel nut powder, mouth fresheners, ice candy, and tabletop sweeteners. Chromatography was performed on silica-gel 60 F254 plates with chloroform-methanol-acetic acid 64:35:1 or acetone-isopropanol-acetic acid 60:39:1 as mobile phases. The bands corresponding to the saccharin were scanned in absorbance mode at 230 nm. The calibration plot showed peak area was a linear function of concentration over the range 250–1250 ng µL−1. The relationship between peak area and the amount of saccharin was evaluated by linear regression analysis. The limits of detection and quantification of saccharin were 40 and 130 ng, respectively. Mean recovery from spiked samples was 102.3% for cola drinks and 98.8% for lemon juices. Relative standard deviation (RSD) for cola drinks, lemon juices, ice candy, mouth freshener, betel nut powders, and tabletop sweeteners were 2.1, 4.2, 3.4, 3.0, 4.9, and 4.1%, respectively. The procedure was validated for analysis of saccharin in these food products.

Determination of cyclamate in urine by derivatized gas chromatography-mass spectrometry

Aim: It is important in toxicological/drug screening work to rule out the possible interfering analytes, to eliminate the false positive or negative results. In this paper, we describe a simple, selective, and sensitive derivatized GC-MS method for the determination of cyclohexylsulfamic acid (cyclamate) in urine. Materials and Methods: Elite- 5MS capillary column was used for the separation of analytes and detection using GC-MS. The analysis was carried out in selected ion monitoring mode (SIM) in the range of 26 to 200 using m/z values of 57, 30, 55, 41, 44, 67, 82, 98, and 39. Results and Discussion: The method is based on the conversion of cyclamate into nitroso derivative of cyclamate followed by its gas chromatography-mass spectrometry determination. The limit of detection, limit of quantitation, and linearity range of the proposed method were found to be 0.2 μg/ ml, 0.7 μg/ml, and 1-15 μg/ml, respectively. The recovery of the present method is in the range of 88-94%. Conclusion: The proposed method can be applied for detection and quantification of cyclamate in urine.