气质联用测定杭白菊等3种中药中5种拟除虫菊酯类农药残留

Five pyrethroid pesticide residues for three kinds of traditional Chinese medicines using GC-MS

采用浊点萃取反萃取样品前处理方法,建立气质联用测定杭白菊Chrysanthemum morifolium,白术Atractylodes macrocephala和山茱萸Cornus officinalis中甲氰菊酯、高效氯氟氰菊酯、氯菊酯、氯氰菊酯和氰戊菊酯等5种拟除虫菊酯类农药残留量的测定方法。选用聚乙二醇6000作为浊点萃取的提取剂,异辛烷为反萃取剂,HP-5MS色谱柱为分析柱,气相色谱质谱法进行检测,外标法计算含量。结果表明：5种拟除虫菊酯类农药在15.00~2 000.00μg·kg-1范围内呈良好的线性关系,相关系数为0.955~0.999,检出限为0.63~3.10μg·kg-1,定量限为2.10~10.31μg·kg-1。3种中药的加标回收率为71.22%~91.00%,相对标准偏差（RSD）为3.20%~8.20%。该方法操作简单、安全,可应用于杭白菊、白术、山茱萸中5种拟除虫菊酯类农药残留的检测。

Methods for residual determination by gas chromatography mass spectrometry （GC-MS） of five pyrethroid pesticides in Chrysanthemum morifolium, Atractylodes macrocephala and Cornus officinalis were established. Cloud point extraction-back extraction was used as sample pretreatment method,and PEG 6000 was used as an extraction agent, isooctane was used as a back-extractant, a chromatographic column HP-5MS was used as an analytical column. Content was calculated by the external standard method using GC-MS. Results showed a linear range from 15.00 to 2 000.00 μg kg-1 with favorable correlation coefficients （r=0.955-0.999）. For the five pyrethroid pesticides, the limit of detection was 0.63-3.10 μg .kg-1 and quantitation was 2.10- 10.31 μg kg-1 At spiked concentrations of 50.00-500.00 μg kg-1, recoveries ranged from 71.22% to 91.00%. This proposed method can be applied to determine pyrethroid pesticide residues in Chrysanthemum morifolium, A. macrocephala, and Comus offwinalis.