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目的建立蔬菜中多种农药残留固相萃取-GC-MS分析方法。方法样品切碎匀浆后加乙腈提取,提取液经Envi-18柱和Carb/NH2柱双重净化,浓缩,正己烷定容,经DB-5MS色谱柱GC-MS法测定,外标法定量。结果各农药组分在0.125μg/mL-1.0μg/mL范围线性关系良好,相关系数≥0.995,加标回收率为67.9%-102.7%,RSD为2.1%-6.2%(n=6),检出限为0.003 mg/kg-0.02 mg/kg。结论方法样品前处理简单,定性定量准确灵敏,能够满足蔬菜中多种农药残留的检测。
Objective To establish a method for the determination of various pesticide residues in vegetables by GC-MS. Methods The samples were homogenized and extracted with acetonitrile. The extracts were purified by Envi-18 column and Carb / NH2 column, concentrated, and fixed in n-hexane. The residue was determined by GC-MS with DB-5MS column and quantified by external standard method. Results The linear range of each pesticide was 0.125μg / mL-1.0μg / mL, the correlation coefficient was ≥0.995, the recovery was 67.9% -102.7% and the RSD was 2.1% -6.2% (n = 6) The limit is 0.003 mg / kg to 0.02 mg / kg. Conclusion The method of sample preparation is simple, accurate and sensitive qualitative and quantitative, and can meet the detection of a variety of pesticide residues in vegetables.