利用氣相層析串聯質譜法及超高效液相層析串聯質譜法同時檢測土壤中352種農藥殘留

Gas chromatography-tandem Mass Spectrometry and Ultra Performance Liquid chromatography-tandem Mass Spectrometry for the Simultaneous Determination of 352 Pesticide Residues in Soil

施念昊(Nien-Hao Shih) ； 許得美(De-Mei Hsu) ； 徐慈鴻(Tsyr-Horng Shyu) ； 初建(Chien Chu)

《臺灣農藥科學》 6期 (2019/06) Pp. 1-36

https://doi.org/10.6671/TPS.201906_(6).01

摘要

作物在耕作期間，為防治病蟲草害會施用不同種類的農藥，因此需要建立多重殘留分析方法，以便同時準確檢測土壤中的農藥殘留，本研究建立之土壤中農藥多重殘留檢測方法，可供未來執行臺灣農田環境中土壤之農藥殘留檢測及環境風險評估。供試土壤樣品以自動索氏萃取法（Soxhlet extraction）進行前處理，萃取液分別以氣相層析串聯質譜儀（GC-MS／MS）及超高效液相層析串聯質譜儀（UPLC-MS／MS），檢測195及157項農藥。GC-MS／MS基質匹配檢量線範圍為5～500μg／L，土壤基質分別添加10及40μg／kg農藥標準品，以GC-MS／MS分析，回收率達64.5～115.6%及60.1～119.1%，相對標準偏差（relative standard deviation，RSD）低於20%。另外，UPLC-MS／MS基質匹配檢量線範圍為2～200μg／L，回收試驗添加濃度為4及20μg／kg，回收率分別達64.3～115.4%及63.6～110.0%，相對標準偏差低於20%。建立之檢測方法參加ERA（Environmental Resource Associates）所舉辦之土壤中有機氯農藥能力測試，20種有機氯農藥皆通過能力測試，顯示此方法亦適用於土壤中有機氯農藥之檢測。

關鍵字

土壤 ； 農藥 ； 氣相層析串聯質譜儀 ； 超高效液相層析串聯質譜儀

並列摘要

Pesticides are applied widely in agriculture to protect plants from disease, weeds, and insect damage. As diverse classes of pesticides exist, conducting a credible risk assessment requires the use of multi-residue methods that allow for pesticide residues to be accurately and simultaneously measured in soil. Accordingly, the purpose of this study was to establish a multi-residue method which is capable of assessing the risk of various pesticides used in agricultural soil. To test the efficacy of our proposed method, we extracted soil samples using automatic Soxhlet extraction. A total of 195 and 157 pesticide compounds were analyzed by GC-MS/MS and UPLC-MS/MS, respectively. The matrix-matched calibration range for GC-MS/MS was 5~500 μg/L, and the average recoveries of the 195 pesticides analyzed by GC-MS/MS at two spike levels (10 and 40 μg/kg) were 64.5~115.6% and 60.1~119.1%, respectively, with relative standard deviations (RSDs) of less than 20%. The matrix-matched calibration range for UPLC-MS/MS was 2~200 μg/L, and the average recoveries of the 157 pesticides analyzed by UPLC-MS/MS at two spike levels (4 and 20 μg/kg) were 64.3~115.4% and 63.6~110.0%, respectively, with RSDs of less than 20%. The established analytical method participated in the proficiency testing of organochlorine pesticides in soil held by Environmental Resource Associates (ERA). Results showed that 20 organochlorine pesticides passed proficiency testing, which also revealed that our proposed method is suitable for the detection of organochlorine pesticides in soil. Therefore, the method is likely to be useful in the analysis and assessment of pesticide residues in agricultural soil.

並列關鍵字

soil ； pesticides ； GC-MS/MS ； UPLC-MS/MS