液相色谱-串联质谱法测定蔬菜、水果中氨基甲酸酯类农药残留量  

LC-MS/MS Determination of Residual Amounts of Carbamate Pesticides in Vegetables and Fruits

作　　者：罗惠明[1] 陈燕勤[1] 梁希扬[1] 张林田[1] 

机构地区：[1]汕头出入境检验检疫局,汕头515031

出　　处：《理化检验（化学分册）》2009年第8期994-997,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：应用液相色谱-串联质谱法测定了蔬菜及水果中10种氨基甲酸酯类农药的残留量。试样用乙腈提取,提取液经转变成甲醇-二氯甲烷(1+99)溶液后用固相萃取法净化。淋出液经氮气吹干后,用1 mL乙腈溶解残渣,所得溶液用于LC-MS/MS测定。测定中用C_(18)色谱柱固定相,用乙腈及甲醇-水溶液以不同比例混合后作为流动相进行梯度淋洗。10种农药的检出限(3S/N)均为1μg·kg^(-1)。在3种不同的浓度水平上(1,10,100μg·kg^(-1))作回收试验,测得椰菜中农药的回收率在78.5%～105.0%之间,橙中农药的回收率在80.3%～106.0%之间,相应测定结果的相对标准偏差(n=6)依次在4.6%～19.8%及3.5%～17.7%范围内。Residual amounts of ten carbarnate pesticides in vegetables and fruits were determined by LC-MS/ MS. Samples of vegetables or fruits were extracted with acetonitrile. Sample solution in CH3OH-CH2Cl2 （1＋99） was purified by SPE and the eluate, after evaporation to near dryness by N2-blowing and dissolution in 1 mL of acetonitrile, was used for LC-MS/MS determination, with Cls chromatographic column and gradient elution using acetonitrile and methanol-water mixed solution as mobile phase. Detection limits （3S/N） for the 10 pesticides found were 1μg· kg^-1. Recovery of the method was tested at 3 concentration levels of 1, 10, 100μg· kg^-1 for each of the 10 pesticides, values of recovery found for savoy were ranged from 78. 5% to 105. 0% and for orange were ranged from 80. 3% to 106. 0%, with values of RSD＇s （n=6） in the ranges of 4. 6%--19. 8% and 3. 5%--17. 7% respectively.

关 键 词：液相色谱-串联质谱法 氨基甲酸酯类农药 蔬菜 水果 

分 类 号：O657.63[理学—分析化学]