气相色谱-质谱法测定蔬菜中65种除草剂的残留量  

Determination of 65 herbicides in vegetables by gas chromatography-mass spectrometry

作　　者：杜晓林[1,2] 荫硕妍[1] 李荷丽[1] 苗虹[1,2] 吴永宁[1,2] 

机构地区：[1]国家食品安全风险评估中心卫生部食品安全风险评估重点实验室,北京100021 [2]中国疾病预防控制中心化学污染与健康安全重点实验室,北京100021

出　　处：《中国食品卫生杂志》2013年第3期241-245,共5页Chinese Journal of Food Hygiene

基　　金：国家科技支撑计划课题(2011BAK10B06)

摘　　要：目的建立蔬菜中65种不同类别除草剂的气相色谱-质谱(GC-MS)检测方法。方法样品用乙腈超声提取后,经Carb/NH2柱净化,采用GC-MS检测,以基质匹配的标准校正曲线外标法定量。结果除卞草唑的线性范围为20～1 000μg/L,其他64种除草剂在10～1 000μg/L范围内呈良好线性,相关系数均大于0.998;各农药的方法检出限为0.02～2.2μg/kg,定量限为0.1～7.4μg/kg;以空白蔬菜样品(选取油菜为代表性基质)进行加标水平为5、10和20μg/kg的加标回收试验,除扑草灭和乙氧苯草胺的回收率在41.1%～59.4%之间外,各除草剂的回收率均在60.9%～117.9%之间,相对标准偏差(RSD)低于14.0%。对9份蔬菜样品(包括土豆、油菜、白菜、菠菜)进行检测,1份样品(白菜)检出氟乐灵,其含量为2.0μg/kg。结论该检测方法快速、简便、准确,适用于蔬菜样品中除草剂类农药残留的检测。Objective To develop a new method for quantitative determination of 65 herbicides belonging to different chemical families in vegetables by gas chromatography-mass spectrometry （GC-MS）. Methods Samples were ultrasonically extracted with acetonitrile and the extracts were cleanuped with Carb/NH2 cartridge before GC-MS analysis. Matrix-matched calibration was used for quantification. Results The linearity was satisfying within the range of 10-1000μg/L, and the coefficients of determination （r） were above 0. 998. The limits of detection （LODs） and the limits of quantification （LOQs） were 0.02 - 2. 2 p,g/kg and 0. 1 - 7.4μg/kg, respectively. The recoveries for spiked samples at the levels of 5, 10 and 20 μg/kg ranged from 60. 9% to 117.9% , except for EPTC and Etobenzanid in the range of 41.1% -59.4%. The relative standard deviations （RSD） were below 14. 0%. Trifluralin was detected in 1 out of 9 vegetable samples collected from local market, with the concentration of 2. 0 μg/kg. Conclusion The proposed method was rapid, simple and sensitive for the analysis of 65 herbicides in vegetables.

关 键 词：气相色谱-质谱(GC—MS) 农药残留 蔬菜 除草剂 

分 类 号：R155.5[医药卫生—营养与食品卫生学]