GC-MS/MS를 이용한 축산물 시료 중 29종 농약의 다성분 분석법 개발

The optimization and validation of multi-residue analysis for 29 pesticides in various meat matrices were evaluated. The developed method was validated in five meat matrices (pork belly, sirloin, chicken drumstick, lard, and beef tallow according to the CODEX guideline in terms of recovery, precision, calibration curve linearity, the limit of quantitation (LOQ) and matrix effect. In this study, meat samples were extracted using a QuEChERS extraction followed by optimization of sample clean-up. The clean-up method was then compared and optimized based on the d-SPE(PSA, C18, Z-SEP) and SPE cartridges(aminopropyl, C18, florisil). For the optimized analysis method, it is suitable to use the SPE cartridge as a clean-up method rather than d-SPE in order to improve the sensitivity of pesticides and reduce the matrix effect. In the clean-up method using the SPE cartridge, the use of the C18 SPE cartridge met most of the pesticide recovery criteria. The results of the optimized method showed that above 85% of pesticides gained the LOQs results of below 0.01 mg/kg, and over 90% of pesticides achieved good calibration curve linearity results (R2 > 0.99). As a result of the recovery test applied in an optimal method, more than 80% of the pesticides in the sample of pork belly, sirloin, and chicken drumstick satisfied recovery and precision criteria. In contrast, in lard and beef tallow, only 65% of pesticides met recovery and precision criteria. Therefore, it was confirmed that the recoveries measurement pesticide depends on the fat content of the samples. It can be seen that this fat content also affects a matrix effect. The average matrix effect was 16.6 ~ 30.7% in the samples of pork belly, sirloin, and chicken drumstick, while the average matrix effect was over 50% in the pork and beef fat sample. Although the matrix effect was different for each pesticide, most of the pesticides were affected by ion enhancement. In conclusion, it is judged that it will be possible to use it as a multi-residue analysis method for 29 pesticides on the meat sample.