Cijo John

DETERMINATION OF CLONAZEPAM IN HAIR AND NAIL USING LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY (LC-MS/MS)

Clonazepam, (5-(2-Chlorophenyl)-7-nitro-1,3-dihydro-1,4-benzodiazepin-2-one), a nitrobenzodiazepine and a scheduled drug, is one of the most highly abused drugs in recent times. A sensitive analytical methodology using Liquid Chromatography tandem Mass Spectrometry (LC-MS/MS) was developed for the determination of clonazepam in human hair and nail samples. The method involves the decontamination of hair and nail using 2 mL each of 0.1% SDS (sodium dodecyl sulfate), water, and methanol, dried followed by incubation in phosphate buffer (pH = 8), extraction with diethyl ether:chloroform (70:30, v/v), separation, and detection using liquid chromatography–tandem mass spectrometry. The method was totally validated with the limit of detection (LOD) of clonazepam estimated as 0.50pg/mg and the limit of quantification (LOQ), 2.0pg/mg of hair and nail. Linearity was observed in the range 2.0 pg/mg to 5000 pg/mg with r2 > 0.9980. The extraction recoveries, intra-day and inter-day precisions, accuracy, and matrix effect were also studied for the developed method. The amount of clonazepam detected in the hair and nail of different subjects was found to be in the range of 0.1156–1.040 ng/mg and 0.0713–0.880 ng/mg, respectively. The method is highly sensitive, precise, and reliable for the determination of clonazepam in hair and nail, which can be adopted by law enforcement laboratories for routine analysis.

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.

Simultaneous Determination of p-Hydroxybenzoate Preservatives in Pharmaceuticals and Personal Care Formulations

A new simple, reliable and selective Thin-Layer Chromatographic (TLC) method has been developed for the simultaneous determination of four common p-hydroxy benzoates (parabens); methyl paraben (MP), ethyl paraben (EP), propyl paraben (PP) and butyl paraben (BP) using mobile phase in basic medium on silica gel F254 stationary phase. Detection was carried out with newly developed chromogenic visualisation reagent. Studies for minimum detection limit of the compounds were performed with new method. The detection limit for all these compounds with new chromogenic visualisation reagent were in the range of 0.4–0.8 (μg/spot). The method gave reproducible results and was successfully applied to simultaneous determination of these compounds in commercially available personal care products and pharmaceutical preparations. The separation method is inexpensive and reliable.