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
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.
氨基甲酸酯类农药
固相萃取
蔬菜和食用菌
UHPLC-MS/MS
Carbamate pesticides
Solid phase extraction
Vegetable and edible mushrooms
Abstract
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%.
中图分类号 O657.63
所属栏目 试验与研究
基金项目 “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)
收稿日期 2009/4/29
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备注蒋施(1978-),女,连云港人,博士,工程师,从事农兽药残留研究.
引用该论文: JIANG Shi,ZHAO Ying,JIN Yan,XU Yi-hong,LIU Yu,ZHONG Yu. UHPLC-MS/MS Determination of Residual Amounts of 19 Carbamate Pesticides in Vegetable and Edible Mushrooms[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(6): 593～597
蒋施,赵颖,金雁,徐宜宏,刘瑜,钟钰. 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[J]. 理化检验－化学分册, 2010, 46(6): 593～597
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