Simultaneous determination of pyrethroids from pesticide residues in porcine muscle and pasteurized milk using GC

• Published in: Journal of separation science Vol. 32; no. 2; pp. 244 - 251
• Main Authors: Khay, Sathya, Abd El-Aty, A. M., Choi, Jeong-Heui, Shin, Eun-Ho, Shin, Ho-Chul, Kim, Jin-Suk, Chang, Byung-Joon, Lee, Chi-Ho, Shin, Sung-Chul, Jeong, Ji Yoon, Shim, Jae-Han
• Format: Journal Article
• Language: English
• Published: Weinheim WILEY-VCH Verlag 01.01.2009; WILEY‐VCH Verlag; Wiley
• Subjects: Animal tissues; Animals; Biological and medical sciences; Electrons; Food Analysis - methods; Food industries; Fundamental and applied biological sciences. Psychology; Gas Chromatography-Mass Spectrometry - methods; Hot Temperature; Meat - analysis; Meat and meat product industries; Milk - chemistry; Milk and cheese industries. Ice creams; Multiresidue; Muscles - chemistry; Pesticide Residues - analysis; Pesticide Residues - chemistry; Pyrethrins - analysis; Pyrethrins - chemistry; Pyrethroids; Simultaneous; Swine; Electron capture detector; Pasteurized milk; Multiresidue; Chemical analysis; Insecticide; Liquid liquid extraction; Coupled method; Pesticides; Pyrethroids; Solvent extraction; Contamination; Gas chromatography; Multicomponent analysis; Sample preparation; Residue; Cypermethrin; Animal tissues; Simultaneous measurement; GC; Simultaneous; Deltamethrin; Mass spectrometry; Pork; Quantitative analysis
• ISSN: 1615-9306; 1615-9314
• DOI: 10.1002/jssc.200800481

The principal goal of this work was to develop an efficient method for the simultaneous determination of four pyrethroid (PYR) insecticides, cyfluthrin, cyhalothrin, cypermethrin, and deltamethrin, in porcine muscle and pasteurized milk using liquid–liquid extraction (LLE). Sample extraction was carried out with and without additional column cleanup procedures, and the final determination was made using GC with electron‐capture detector (ECD). The pesticide identity was confirmed using GC‐MS in the SIM mode. Since there were minor differences between the extraction procedures, extraction without the additional cleanup procedure was used throughout the work. The method was validated by fortifying blank samples with half, two, and four times the maximum residue limit (MRL) of each PYR. The average recoveries (n = 6) ranged from 83.5 to 99.2% and 82.9 to 109% in porcine muscle and pasteurized milk, respectively. The repeatability of measurements expressed as RSDs, was in the range of 1.7–11.9 and 1.5–10.3% in porcine muscle and pasteurized milk, respectively. The LODs ranged from 3.3 to 9 and 3 to 8.1 ppm, whereas the LOQs ranged from 10 to 27.4 and 9 to 24.6 ppm, in porcine muscle and pasteurized milk, respectively. The applicability of the method was demonstrated by analyzing real samples collected from major cities in the Republic of Korea. No residues of the selected pesticides were detected in any of the samples.