石英毛细管气相色谱法测定柘荣太子参中联苯菊酯、毒死蜱的农药残留量

目的:建立柘荣太子参中联苯菊酯、毒死蜱的农药残留量的测定方法。方法:以盐析法提取,柱层析法净化,以石英毛细管气相色谱法,程序升温,ECD检测器,测定2种农药的残留量。结果:联苯菊酯在0.041~2.466 μg·mL^-1,毒死蜱在0.021~1.254 μg·mL^-1范围内呈现良好的线性关系,相关系数分别为0.9999、0.9995;平均回收率分别为88.3%、83.5%,RSD均小于4.5%(n=3)。结论:该法简便、快速、准确,可作为太子参中联苯菊酯、毒死蜱农药残留量的检测方法。

Objective: To establish a method to determine the quantity of the residual of bifenthrin anc chlorpyrifos in the Zherong Pseudostellaria tererophylla.Methods: The sample was extracted by using salting out method and purified by column chromatography.The temperature was programmed,and ECD detector was used.The quantity of the residual of bifenthrin anc chlorpyrifos was calculated according to the external standard method.Results: The results showed a good linear relationship for bifenthrin when the concentration was in the range of 0.041-2.466 μg·mL^-1(r=0.9999).It also showed a good linear relationship for chlorpyrifos when its concentration ranged between 0.021-1.254 μg·mL^-1(r=0.9995).The average recovery rates for bifenthrin anc chlorpyrifos were 88.3% and 83.5%,respectively.The RSD were both less than 0.45%(n=3).Conclusion: The method is simple,rapid and accurate,thus it is proposed to be used to determine the quantity of the residual of bifenthrin and chlorpyrifos.

1 The People's Republic of China Ministry of Health,Bureau of Pharmaceutical Affairs Bureau(中华人民共和国卫生部药政管理局).Modern Practical Materia Medica(VolumeⅠ)(现代实用本草上册).Beijing(北京):People's Medical Publishing House(北京人民卫生出版社),1997 .138
2 ChP(中国药典).2010.VolⅠ(一部):63
3 DU Dao-ling(杜道林),GAN Bing-chun(甘炳春),WANG You-sheng(王有生).Standardization cultivation of Arecacatechul catechu L.and standard operation practice of pretection tending(槟榔规范化种植与保护抚育标准操作规程的研究).Res Pract Chin Med(现代中药研究与实践),2005,19(3):18
4 YANG Xiu-wei(杨秀伟),WANG Ying(王莹).Myristica fragrans in heavy metals and pesticide residues(肉豆蔻中重金属和农药残留量分析).Chin J Pharm Anal(药物分析杂志),2007,27(10):1517
5 ZHANG Ya-li(张亚莉),YAN Zheng(阎正).Progress of the technology for pesticide residue analysia in herbal medicines(中药中农药残留分析技术进展).Hebei J Ind Sci Technol(河北工业科技),2004,21(5):56
6 DAI Bo(戴博),JIN Hong-yu(金红宇),TIAN Jin-gai(田金改).Progress achieved in determination method of extrinsic harmful residues in traditional Chinese medicine(中药中外源性有害残留物检测方法研究进展).Chin J Pharm Anal(药物分析杂志),2008,28(6):1016
7 GAO Meng-nan(高梦南),WANG Yan-ping(王燕萍),TANG Hong-wei(唐红卫),Application of gel permeation chromatography to cleaning up soil extracts in determination of organochlorine pesticides(凝胶渗透色谱净化在土样有机氯测定中的应用).Environ Sci Technol(环境科学与技术),2006,29(3):38
8 ChP(中国药典).2010.VolⅠ(一部):Appendix(附录)57
9 LI Jin-jia(黎金嘉)Microemulsion technology development of Uranus(用微乳技术开发天王星).Pest Market News(农药市场信息),2004,233:33
10 JIAO Li-fei(焦利飞),YAN Chang-hui(闫长会),ZHAO Jun(赵君).Reproductive toxicity of low-level chlorpyrifos repeated exposure and its mechanisms in male rats(低剂量毒死蜱重复染毒诱发雄性大鼠生殖毒性及其机制).Chin J Pharmacol Toxicol(中国药理学与毒理学杂志),2011,25(6):568
11 WENG Shu-qin(翁淑琴),YOU Yong-ji(游勇基).SPE-HPLC determination of pyrethroid pesticide residues in Platycodon grandiflorum(固相萃取-高效液相色谱法测定桔梗中拟除虫菊酯的农药残留).Chin J Pharm Anal(药物分析杂志),2011,31(9):1818