A simple, rapid, cost‐effective and environment friendly analytical method based on dispersive liquid‐liquid microextraction (DLLME) coupled to injection port silylation (IPS)–gas chromatography‐mass spectrometry is described for the determination of morphine in illicit opium samples. Raw opium was dispersed in ultrapure water and 5 mL of aqueous sample was subjected to DLLME by rapidly injecting a mixture of chloroform and acetone (extraction and disperser solvent, respectively) followed by ultrasonication for 1 min and subsequent centrifugation for 3 min at 5000 rpm. The sedimented phase thus obtained was reconstituted in acetonitrile and 1 µL along with 1 µL of N,O‐Bis(trimethylsilyl)acetamide (BSA) was injected manually into GC‐MS injection port at a temperature of 250°C. The derivatization reaction was completed instantaneously inside the heated GC‐MS injection port without any side product. Various parameters associated with IPS and DLLME have been thoroughly optimized. Under the optimized conditions, the method has been found linear in the range of 5‐50 µg/mL with a correlation coefficient (R2) of 0.997. The limit of detection (LOD) and limit of quantification (LOQ) for morphine‐diTMS were found to be 1.6 and 4.8 µg/mL. The method has been successfully applied for the quantitative analysis of morphine in illicit opium samples. In conclusion, the proposed method has completely eliminated the time consuming and laborious steps of LLE and in‐vial silylation and can be routinely used for analysis of opium and other polar analytes in forensic science laboratories.

Background: Fruits and vegetables are daily staple food of human community. It is important to include fruits and vegetables in our daily diet to remain healthy and active. Even though fruits and vegetables are healthy, but they are equally prone to pests and diseases which attack them during their time of production as well as storage, thus, degrading their yield and quality. So, to prevent these issues farmers use high amount of pesticides and other products, this enters in our body orally. A large amount of pesticides gets removed from the human body in the form of urine and fecal matter but, still some pesticides (especially chlorpyrifos) are very persistent and can remain in human body for a long term. This study aims at the presentation of a method for the determination of chlorpyrifos from grapes sample by TLC-FID technique. The residue of pesticides was extracted from the sample in ethyl acetate. The grapes sample was macerated, extracted, filtered and analyzed by the proposed method. The analyzed sample showed chlorpyrifos contamination even in the lowest amount taken for analysis. Results: The TLC-FID technique using mobile phase consist of hexane: acetone (9:1, v/v)has been found to be more effective and less tedious as chromarods were used for performing chromatographic separation. Chlorpyrifos were extracted from the samples by liquid-liquid extraction before the analysis. The method developed can be used to detect chlorpyrifos residues in a concentration as minimum as 0.02 mg/Kg.

Background Recent advances in the diversified anti-diabetic drugs have appeared in the startling increase in the count of poisoning cases. The epidemics of diabetes mellitus are increasing; hence, the no. of anti-diabetic drug users raised by 42.9%. The use of glimepiride raised to 24%. As the toxicity and drug cases are also escalating with increasing epidemics of diabetes mellitus, a novel gas chromatography-mass spectrometry (GC-MS) method for detecting glimepiride in biological matrices is developed. Results Liquid-liquid extraction method was employed by using 1-butanol: hexane (50:50, v/v) under an alkaline medium, and then back extraction was done via acetic acid. Distinct derivatization techniques were employed for the sample preparation for GC-MS analysis, i.e., silylation and acylation. Derivatization approaches were optimized under different parameters, i.e., reaction temperature and reaction time. N-Methyl-N-(trimethylsilyl) trifluoroacetamide [MSTFA] was found to be the best sound derivatization reagent for the GC-MS analysis of glimepiride. Total ion current (TIC) mode was selected for the monitoring of ions of trimethylsilyl (TMS) derivative of glimepiride with an m/z ratio of 256. Distinct parameters like specificity, carryover, stability, precision, and accuracy were evaluated for validating the identification method. The GC-MS method is found to be linear and illustrated within the range 500 to 2500 ng/ml with the value of R2 (coefficient of determination) at 0.9924. The stability of the extracted and derivatized glimepiride was accessed with regard to processed/extracted sample conditions and autosampler conditions, respectively. Accuracy at each concentration level was within the + 15% of the nominal concentration. Precision (%) for the interday and intraday analysis was found to be in the respectable spectrum. Conclusion Henceforth, the proposed GC-MS method can be employed for the determination of glimepiride in biological matrices.