摘要
目的建立固相萃取-气相色谱质谱内标法同时测定茶叶中噻螨酮和喹螨醚农药。方法采用乙腈提取,经DIKMA Pro Elut TPC固相萃取柱净化,以混合溶剂乙腈-甲苯(3∶1,V/V)洗脱,减压蒸馏浓缩,经HP-5MS毛细管柱程序升温分离,质谱检测器检测,全扫描模式定性,选择离子模式定量测定。结果噻螨酮和喹螨醚在0.1 mg/kg^10 mg/kg和0.01 mg/kg^1 mg/kg浓度比值与峰面积比值呈良好线性关系,相关系数分别为0.996 8和0.999 1,方法检出限分别为0.016 mg/kg和0.002 mg/kg(S/N=10),高、中、低3个浓度进行了加标回收添加实验,平均加标回收率为70.1%~105.2%,方法精密度以6次测定值的RSD表示,RSD为2.6%~9.8%。用该方法对10个茶叶样品进行分析,均未检出噻螨酮和喹螨醚。结论该方法灵敏度高,回收率好,专属性强,能快速准确测定茶叶中噻螨酮和喹螨醚。
Objective To develop a method for simultaneously determining the concentrations of hexythiazox and fenazaquin pesticides in tea by solid phase extraction-gaschromatographic mass spectrometry（GC-MS） with interal standard method.Methods The pesticides were extracted from tea with acetonitrile and the extract was cleaned up with DIKMA Pro Elut TPC SPE column and eluted with acetonitrile-toluene（3∶1,V/V）. After vacuum distillation concentration,the extracts were separated on HP-5 MS capillary column programmed temperature and detected qualitatively by mass spectrometer with scan mode and detected quantitatively with SIM mode. Results Good linear relationships were obtained in the range of 0. 1 mg/kg-10 mg/kg for hexythiazox and in the range of 0. 01 mg/kg-1 mg/kg between concentration ratio and peak area ratio for fenazaquin,and the correlation coefficients（r） of the calibration curve were 0. 996 8 and 0. 999 1,respectively. The detection limits were 0. 016 mg/kg for hexythiazox and 0. 002 mg/kg for fenazaquin,respectively. The recoveries at high,middle,and low concentrations ranged from 70. 1% to 105. 2%. The precision of the method was showed by RSD（n = 6）,which ranged from 2. 6%to 9. 8%. The method was applied to 10 samples,but hexythiazox and fenazaquin pesticides were not detected. Conclusion The method is high sensitive with high recovery. It can be specifically used to detect hexythiazox and fenazaquin pesticides in tea quickly and accurately.
作者
王秀丽
贾彦博
李玮
马慧丽
胡程
WANG Xiu-li;JIA Yan-bo;LI Wei;MA Hui-li;HU Cheng(Hangzhou Institute for Food and Drug Control,Hangzhou,Zhejiang 310022,China)
出处
《中国卫生检验杂志》
CAS
2018年第15期1817-1820,共4页
Chinese Journal of Health Laboratory Technology
关键词
固相萃取
气相色谱质谱法
茶叶
噻螨酮
喹螨醚
Solidphase extraction
Gaschromatographic mass spectrometry
Tea
Hexythiazox
Fenazaquin
作者简介
王秀丽（1976-），女，硕士，高级工程师，主要从事食品，检测与研究。
