大黄的HPLC指纹图谱及禁用农药的残留研究
投稿时间:2023-10-30  修订日期:2024-05-06  点此下载全文
引用本文:毛泽玲,文波.大黄的HPLC指纹图谱及禁用农药的残留研究[J].药学实践杂志,2024,42(7):297~304,314
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作者单位E-mail
毛泽玲 浙江省桐庐县中医院, 浙江 杭州 311500  
文波 浙江桐君堂中药饮片有限公司, 浙江 杭州 311500 wenborin@126.com 
基金项目:杭州市卫生科技计划项目(B20210302)
中文摘要:目的 建立不同种大黄的HPLC特征指纹图谱和禁用农药残留检测方法,并综合评价其药材质量。方法 收集3种大黄共20批,采用HPLC法进行分析,流动相为甲醇-0.1 %磷酸溶液;梯度洗脱;柱温35 ℃;检测波长254 nm;流速1.0 ml/min;并对结果进行聚类分析。采用直接提取法,并建立HPLC-串联质谱法,气相色谱-串联质谱法,对不同来源、产地大黄的33种禁用农药进行检测。结果 掌叶大黄、唐古特大黄、药用大黄3种来源大黄的指纹图谱与其对照指纹图谱的相似度均>0.95,聚类分析将20批大黄样品分为3类。不同产地的大黄样品均未检出33种禁用农药。结论 3种大黄药材质量差异较大,建立的HPLC指纹图谱和禁用农残的方法稳定、可靠、简便准确,可以为大黄的质量控制评价提供依据。
中文关键词:大黄|指纹图谱|禁用农药残留
 
HPLC fingerprint of Radix Rhubarb and forbidden pesticide residues
Abstract:Objective To establish the HPLC fingerprint and pesticide residue detection methods for different kinds of rhubarb, and evaluate the quality of rhubarb comprehensively. Methods 20 batches of three types of rhubarb were collected and analyzed by high-performance liquid chromatography. The mobile phase was methanol-0.1 % phosphoric acid solution; gradient elution; column temperature of 35 ℃; detection wavelength of 254 nm; flow rate 1.0 ml/min. And cluster analysis was performed on the results. Direct extraction method was used and high-performance liquid chromatography-tandem mass spectrometry and gas chromatography-tandem mass spectrometry were established, 33 prohibited pesticides from different sources and origins of rhubarb were detected. Results The similarity among the fingerprint spectra of three sources of rhubarb, namely Rheum palmatum L., Rheum tanguticum Maxim.ex Balf., and Rheum officinale Bail1., and their control fingerprint spectra was>0.95. 20 batches of rhubarb samples were divided into 3 categories by cluster analysis. 33 prohibited pesticides were detected in rhubarb samples from different regions. Conclusion The quality of three kinds of rhubarb was significantly different. The established HPLC fingerprint and the method of banning agricultural residues were stable, reliable, simple and accurate, which could provide a basis for quality control evaluation of rhubarb.
keywords:rhubarb|fingerprint|forbidden pesticide residues
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