固相萃取-气相色谱-质谱联用法测定卷心菜粉中联苯菊酯  

Determination of bifenthrin in cabbage powder by gas chromatography-mass spectrometry with solid phase extraction

作　　者：朱亚娟[1] 李红叶[1] 左迪晓雪 美丽克[1] 

机构地区：[1]新疆生产建设兵团疾病预防控制中心,新疆乌鲁木齐830002

出　　处：《中国卫生检验杂志》2017年第11期1536-1538,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立固相萃取-气相色谱-质谱联用(SPE-GC-MS)测定卷心菜粉中联苯菊酯的方法。方法卷心菜粉样品经固相萃取前处理技术进行提取净化。选择乙腈进行超声浸提,经过弗罗里硅土固相萃取柱净化,有效降低了样品基质带来的背景干扰。采用TR-5MS(30 m×0.25 mm,0.25μm)色谱柱程序升温,GC-MS的离子扫描(SIM)模式检测,选择m/z 181、182、166、165作为特征离子,通过外标法定量。结果联苯菊酯浓度为0.03 mg/L^0.90 mg/L时,基质匹配工作曲线线性关系良好,相关系数为0.999 7;在高、低2种浓度添加水平下,方法的平均加标回收率为98.6%~101%,相对标准偏差(RSD)为2.62%~3.08%;该方法的检出限(LOD,S/N=3)为0.006 mg/kg。结论本方法操作简单、快速,重现性较好,灵敏度和准确度均能满足测定卷心菜粉中联苯菊酯的要求。Objective To establish a method to detect bifenthrin in cabbage power by gas chromatography - mass spectrometry with solid phase extraction（SPE）. Methods The sample was extracted and purified using SPE method. The bifenthrin in sam- ple was extracted with acetonitrile by ultrasonic, and then directly purified by using florisil solid phase extraction column, which effectively reduced the background interference caused by sample matrix. The sample was separated by TR - 5MS （30 m × 0.25 mm, 0.25μm） column with temperature programming, and detected in SIM mode. The ions whose m/z = 181, 182, 166 and 165 were selected as characteristic ions. The external standard curve was used for quantification. Results When the bifenthrin concentration was within 0.03 mg/L - 0.90 mg/L, good matrix matching curve relationship was obtained, and the coefficient of correlation（r） was 0. 999 7. The average recoveries ranged from 98.6% to 101% and the relative standard deviation （RSD） ranged from 2.62% to 3.08% under two kinds of standard addition levels. The limit of detection （LOD, S/N = 3 ） of this method was 0. 006 mg/kg. Conclusion This method is simple, fast, with good reproducibility, sensitive and accurate. It meets the criteria of methodology in the determination of bifenthrin in cabbage power.

关 键 词：固相萃取 气相色谱-质谱联用法 联苯菊酯 

分 类 号：O657.63[理学—分析化学]