Development of a Novel Method for Detection of 54 Pesticides by GCMS/MS-TQD

• Published in: Oriental journal of chemistry 2015, Vol.31 (3), p.1663-1672
• Main Authors: Harinathareddy, A., Prasad, N. B. L, Devi, K., Ravindranath, D
• Format: Article
• Language: English
• Subjects: Acetonitrile; Calibration; Chromatography; Fruits; Fungicides; Gas chromatography; Herbicides; Insecticides; Linearity; Organic chemistry; Pesticides; Phosphates; Regression analysis; Sodium; Sodium chloride; Standard deviation; Toluene; Vegetables
• ISSN: 0970-020X; 2231-5039
• DOI: 10.13005/ojc/310345

Developed Multi residue method for 54 pesticides on GC-MS/MS-TQD (Brukers 436 GC). Organo Chlorines (OCs), Organo Phosphates (Ops), Synthetic Pyrethroids (SPs), Herbicide and Fungicide mixtures of standards supplied by Dr.Ehrenstorfer and sigma Aldrich were prepared in (1:1) Hexane: Toluene (Merck). Eight different concentrations of standards i,e 0.05, 0.1, 0.15, 0.20, 0.25, 0.30 ppm were prepared and injected six replications into GC-MS/MS-TQD. Linearity curve was drawn for each pesticide and Regression values were calculated. Regression value ranged from 0.991-0.999 and percentage of Relative standard deviation is in between 0.29 to 6.14 for the all Organo chlorines. For Organo phosphates Regression value ranged from 0.991-0.999 and percentage of Relative standard deviation is in between 0.31-6.02. For Synthetic pyrethroids Regression value ranged from 0.991-0.999 and percentage of Relative standard deviation is in between 0.58-8.24. For Herbicides, Fungicides and other Pesticides Regression value ranged from 0.994-0.999 and percentage of Relative standard deviation is in between 0.77-3.79. Study the residues of 54 pesticides in vegetables recovered from the developed method been validated for the extraction of pesticides of various chemical classes from vegetables such as tomato. Mixtures of 54 pesticides amenable to gas chromatography were quantitatively recovered from spiked tomato determined by using gas chromatography– Mass spectroscopy. The sample preparation approach is known as QuEChERS, which stands for “quick, easy, cheap, effective, rugged and safe”. As expected, the results are excellent and showed overall average of 98% recoveries with 10% RSD. The method involved extraction with acetonitrile, liquid–liquid partition with addition of NaCl followed by MgSO4 and Primary secondary amine (PSA) and the analyses were carried out with GC–MS equipment. It was a rapid, simple and cost effective procedure. The spiking levels for the recovery experiments were 0.05, 0.25, 0.5 mg kg−1. Adequate pesticide quantification and identity confirmation were done. The recovery ratios, the very good accuracies and precisions, as well as the good matches between the observed ion ratios. the percent recovery of OCs in the range of 83.65%–102.92% in 0.05 mg/kg, in the range of 78.78–99.66% in 0.25 mg/kg.and in the range of 81.18–108.50% in 0.5 mg/kg respectively The percent recovery of OPs in the range of 81.45–100.60% in 0.05 mg/kg, in the range of 81.27–103.72% in