超高效液相色谱-串联质谱法测定蔬菜和食用菌中19种氨基甲酸酯农药残留量  

UHPLC-MS/MS Determination of Residual Amounts of 19 Carbamate Pesticides in Vegetable and Edible Mushrooms

作　　者：蒋施[1] 赵颖[1] 金雁[1] 徐宜宏[1] 刘瑜[1] 钟钰[1] 

机构地区：[1]沈阳出入境检验检疫局,沈阳110016

出　　处：《理化检验（化学分册）》2010年第6期593-597,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金："十一.五国家科技支撑计划"课题"农药与兽药残留确证检测技术研究"中的分课题(2006BAK02A08-005)

摘　　要：采用超高效液相色谱-串联质谱法测定蔬菜和食用菌中19种氨基甲酸酯类农药残留量。样品用丙酮-乙腈(85+15)混合溶剂提取,过PSA固相萃取柱净化,将淋出液蒸发浓缩后用甲醇-水(2+8)混合溶液定容。通过Waters C18色谱柱分离,流出液供串联质谱测定,同位素内标法定量。19种氨基甲酸酯农药的质量浓度与其峰面积和内标物峰面积的比值之间在一定的浓度范围内均呈线性关系。蔬菜和食用菌中19种氨基甲酸酯农药的回收率在71.8%～94.3%之间,相对标准偏差(n=5)在2.36%～13.23%之间。Ultra-high pressure liquid chromatography in hyphenation with tandem mass spectrometry（UHPLC-MS/MS） was applied to the determination of residual amounts of 19 kinds of carbamate pesticides in vegetable and edible mushrooms.The sample was extracted with acetone-acetonitrile（85＋15） solution,which was concentrated and purified by PSA solid-phase extraction column.The eluate was evaporated to near dryness and diluted to a definite volume with methanol-water（2＋8） solution,and separated on the Waters C18 column.The eluate was used for tandem MS analysis.Internal standard calibration of isotope was adopted in the determination.Linear relationships between values of ratio of peak areas of the unknown pesticide to the internal standard and mass concentration of 19 kinds of carbamate pesticides were obtained in the definite ranges.Values of recovery of 19 kinds of carbamate pesticides in vegetable and edible mushrooms were in the range of 71.8%-94.3% and values of RSD′s（n=5） were in the range of 2.36%-13.23%.

关 键 词：超高效液相色谱-串联质谱 氨基甲酸酯类农药 固相萃取 蔬菜和食用菌 

分 类 号：O657.63[理学—分析化学]