气相色谱法测定中药材中菊酯类农药残留的研究

目的为了更加有效测定中药材中拟除虫菊酯类农药的残留量,采用气相色谱法检测,固相萃取净化的分析方法,提高药材的用药安全性。方法在临海市各个药材公司购置主要为药厂提供的中药材品种,每个品种选择3~5个批号,共计150个样品,经提取净化后采用气相色谱法(GC-ECD)测定,可同时测定6种拟除虫菊酯类农药残留量。结果 6种拟除虫菊酯类成分均有检出,检出率为34. 51%,农药的残留含量主要在0. 01~0. 05mg/kg之间,合格率为85. 23%;中药材中6种拟除虫菊酯类农药的平均回收率在83. 14%~103. 81%之间,相对标准偏差(RSD)为4. 0%~6. 4%,6种拟除虫菊酯类农药的线性范围在0. 02~0. 84mg/L之间;最低检测限范围为15. 8~26. 3ng/kg,定量限范围为52. 8~88. 4ng/kg。结论气相色谱法用于拟除虫菊酯类农药残留的检测,对于成分的分离效果好,灵敏度高,指标满足农药残留分析检测的要求,可以为中药材中拟除虫菊酯类农药残留的限量制定提供有效的数据参考。

Study of the determination of pyrethroid pesticide residues in traditional Chinese medicine by gas chromatography

Objective To determine the residual amount of pyrethroid pesticides in Chinese medicinal materials more effectively and improve the safety of medicinal materials,establish an analytical method for gas chromatography and solid phase extraction purification. Methods All kinds of Chinese herbal medicines provided by major pharmaceutical companies in Linhai were purchased,and 3 to 5 batch numbers were selected for each variety,totaling 150 samples. After extraction and purification,they were determined by gas chromatography( GC-ECD). The amount of six pyrethroid pesticide residues was determined. Results All the pyrethroids were detected,the detection rate was 34. 51%,the residual content of pesticides was mainly between 0. 01 and 0. 05 mg/kg,and the pass rate was 85. 23%. The average recoveries of pesticides for 6 pyrethroids in Chinese herbal medicines ranged from 83. 14% to 103. 81%,and the linear range of six pyrethroid pesticides ranged from 0. 02 to 0. 84 mg/L. The detection limit quantitation ranged from 15. 8 to 26. 3 ng/kg,and the limit of quantitation ranged from 52. 8 to 88. 4 ng/kg. Conclusion Gas chromatography is used for the detection of pyrethroid pesticide residues. It has good separation effect and high sensitivity. The index meets the requirements of pesticide residue analysis and detection. The test data can provide an effective data reference for the limit of quantitation for pyrethroid pesticide residues in Chinese herbal medicines.