中药黄芪中8种有机氯农药残留气相色谱分析及其检测结果研究
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摘要
目的研究中药黄芪中8种有机氯农药残留气象色谱分析以及检测结果。方法从我省三级甲等医疗机构采集8份黄芪样品并收集黄芪的产地等信息,按照《中国药典》中的有机氯农药残留气相色谱检测方法,中药黄芪经过粉碎以后使用有机溶剂提取以及磺化后,再使用分流进样的方法经过两次程序升温技术分离,最后使用电子捕获检测器检测并使用外标法计算有机氯农药残留含量。结果在本次的研究中,保留时间最长的农药为pp′-DDT,农药α-BHC的检测浓度最低;使用配备了电子捕获器的气相色谱仪绘制8种有机氯农药的气相色谱图,出峰时间最早的是α-BHC,最晚的是pp′-DDT;在本次实验中,称取黄芪并加入标准品溶液,用所添加的标准溶液为标准,使用外标法定量,计算黄芪的回收率和精密度,其中β-BHC的回收率最低,δ-BHC的精密度最大。结论在对中药黄芪中8种有机氯农药残留的检测中,气象色谱分析方法较好,为安全用药提供了保障,对其他此类中药农药残留问题提供了参考价值,可以进一步的推广。
Objective To study the meteorological chromatographic analysis and detection results of eight organochlorine pesticides in Radix Astragali. Methods Collected 8 samples of Astragalus membranaceus from provincial level A medical institutions and collected information on the origin of Astragalus membranaceus. According to the GC method for organochlorine pesticide residues in the Chinese Pharmacopoeia, the Chinese medicine Astragalus membranaceus was used to extract organic solvents after being crushed and After sulfonation, it was separated by two-time temperature-programming technique using a split injection method. Finally, an electron capture detector was used to detect and use an external standard method to calculate the residual content of organochlorine pesticides. Results In this study, the pesticide with the longest retention time was pp ′-DDT,and the detection concentration of pesticide α-BHC was the lowest; gas chromatograms of eight organochlorine pesticides were drawn using a gas chromatograph equipped with an electron trap. The earliest peak time is α-BHC, and the latest is pp ′-DDT. In this experiment, we took astragalus and added the standard solution. We used the standard solution as a standard and quantified using external standard method. The recovery and precision of Astragalus membranaceus were calculated, among which β-BHC had the lowest recovery rate and δ-BHC had the highest precision.Conclusion The method of meteorological chromatographic analysis was better in the determination of eight organochlorine pesticide residues in Astragalus membranaceus, which provided a guarantee for safe drug use. It provided a reference value for other pesticide residues of traditional Chinese medicine and could be further promoted.
Objective To study the meteorological chromatographic analysis and detection results of eight organochlorine pesticides in Radix Astragali. Methods Collected 8 samples of Astragalus membranaceus from provincial level A medical institutions and collected information on the origin of Astragalus membranaceus. According to the GC method for organochlorine pesticide residues in the Chinese Pharmacopoeia, the Chinese medicine Astragalus membranaceus was used to extract organic solvents after being crushed and After sulfonation, it was separated by two-time temperature-programming technique using a split injection method. Finally, an electron capture detector was used to detect and use an external standard method to calculate the residual content of organochlorine pesticides. Results In this study, the pesticide with the longest retention time was pp ′-DDT,and the detection concentration of pesticide α-BHC was the lowest; gas chromatograms of eight organochlorine pesticides were drawn using a gas chromatograph equipped with an electron trap. The earliest peak time is α-BHC, and the latest is pp ′-DDT. In this experiment, we took astragalus and added the standard solution. We used the standard solution as a standard and quantified using external standard method. The recovery and precision of Astragalus membranaceus were calculated, among which β-BHC had the lowest recovery rate and δ-BHC had the highest precision.Conclusion The method of meteorological chromatographic analysis was better in the determination of eight organochlorine pesticide residues in Astragalus membranaceus, which provided a guarantee for safe drug use. It provided a reference value for other pesticide residues of traditional Chinese medicine and could be further promoted.
引文
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[8]李芳,李钦,顾志荣,等.基于FTIR的黄芪药材产地鉴别及预测研究[J].天然产物研究与开发,2016,13(11):1712-1717.
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[11]国家药典委员会.中国药典一部[M].北京:中国医药科技出版社,2015.
[2]刘德旺,谷彩梅,杨庆珍,等.内蒙古地区道地药材蒙古黄芪资源调查及产地适宜性[J].应用生态学报,2016,27(3):838-844.
[3]Jiao J,Gai QY,Wang W,et al.Enhanced astragaloside production and transcriptional responses of biosynthetic genes in Astragalus membranaceus,hairy root cultures by elicitation with methyl jasmonate[J].Biochemical Engineering Journal,2016,105(12):339-346.
[4]闫嵩,任伟超,刘振鹏,等.黄芪中药种衣剂对黄芪部分生理指标的影响[J].东北林业大学学报,2016,44(2):11-14.
[5]Auyeung KK,Han QB,Ko JK.Astragalus membranaceus:A Review of its Protection Against Inflammation and Gastrointestinal Cancers[J].American Journal of Chinese Medicine,2016,44(1):1-22.
[6]刘德旺,龚苏晓,朱雪瑜,等.蒙古黄芪药材、生饮片及其炮制品质量差异性研究[J].中草药,2016,47(6):905-910.
[7]李欣,王晓萍.气相色谱法测定红霉素残留有机溶媒方法验证[J].当代医学,2009,15(13):79-81.
[8]李芳,李钦,顾志荣,等.基于FTIR的黄芪药材产地鉴别及预测研究[J].天然产物研究与开发,2016,13(11):1712-1717.
[9]熊一峰,秦雪梅,李科,等.从黄芪化学成分测定分析药材商品品规的合理性[J].中草药,2016,47(12):2194-2198.
[10]胡爱萍,李娜.中药处方分析及其在药学服务中的应用研究[J].当代医学,2017,23(8):143-145.
[11]国家药典委员会.中国药典一部[M].北京:中国医药科技出版社,2015.