摘要
本研究旨在建立电感耦合等离子体质谱法(ICP-MS)测定盆消灌肠液(Penxiao enema solution,PES)中5种重金属元素残留量的方法,并提出对该制剂进行安全性评估的模式。以锗(72Ge)、铟(115In)、铋(209Bi)为内标,待测元素对照品为标准物质,采用ICP-MS法对微波消解处理后样品进行Cu、As、Cd、Hg和Pb等5种重金属元素的残留量进行测定;对结果进行聚类分析、方差分析、主成分分析及正交偏最小二乘法判别分析(OPLS-DA),再以单因子污染指数法和内梅罗综合污染指数法对其进行安全性评估,并对重金属残留量和综合污染指数进行Pearson相关性分析。全部样品重金属残留量均符合《中国药典》2020版要求;聚类分析结果表明,15批次样品聚为2类,未检出Hg和Pb元素残留量的样品多聚为一类,主成分分析共提取3个主成分,代表了制剂中80.323%的信息量,15批次样品综合得分范围为-0.616~0.863,以N15综合得分最高,其质量最优,与聚类分析结果基本吻合,综合评分较高的多聚为一类;将2个聚类样品分为A、B、C共3组并进行方差分析,结果表明,Cu元素残留量以A组最低,并与B组、C组均呈现显著性差异,B组、C组相互间无统计学差异,3组中As元素、Cd元素均无统计学差异;OPLS-DA结果表明,Cd、Cu和Hg元素可能是影响制剂质量的关键元素,应予以关注;安全性评价中单因子污染指数范围为0.0000~0.1022,均小于1,综合污染指数范围为0.0130~0.0745,均小于0.7,全部样品均处于安全级。本试验所建立方法准确性高、重复性好、稳定可靠,为制剂提供了一种新的安全性评价模式,可为其药效物质基础研究和临床安全用药提供科学依据。
To establish an inductively coupled plasma mass spectrometry(ICP-MS)method for the determination of 5 heavy metals residues in Pengxiao enema solution(PES),and to propose a model for the safety assessment of the preparation for the first time.The germanium(72Ge),indium(115In)and bismuth(209Bi)as internal standards and reference materials as reference materials,the residual amounts of Cu,As,Cd,Hg and Pb in the samples after microwave digestion were determined by ICP-MS method.The results were analyzed by cluster analysis,analysis of variance,principal component analysis,orthogonal partial least squares-discriminant analysis(OPLS-DA),and then the safety was evaluated by single factor pollution index method and Nemero comprehensive pollution index method.Pearson correlation analy-sis was used to analyze the correlation between heavy metal residues and comprehensive pollution index.The heavy metal residues in all samples met the requirements of Chinese Pharmacopoeia(2020 edition).The results of cluster analysis showed that 15 batches of samples were clustered into two categories,and the samples with no detectable Hg and Pb residues were mostly clustered into one category.A total of 3 principal components were extracted by principal component analysis,representing 80.323%of the information content in the prepara-tion.The comprehensive scores of 15 batches of samples ranged from-0.616 to 0.863.The comprehensive scores of N15 were the highest and its quality was the best,which was basically consistent with the results of cluster analysis.The two cluster samples were divided into three groups A,B and C,and the results of variance analysis showed that the residual amount of Cu in group A was the lowest,showing a significant difference with group B and group C.There was no significant difference between group B and group C.There was no significant difference between group B and group C.There was no significant difference in As and Cd among the three groups.The results of OPLS-DA showed that Cd,Cu and Hg.In the safety evaluation,the single factor pollution index ranged from 0.0000 to 0.1022,all of which were less than 1,and the comprehensive pollution index ranged from 0.0130 to 0.0745,all of which were less than 0.7,All samples were in the safety level.The established method has high accuracy,good repeatability,stability and reliability,and provides a new safety evaluation model for the preparation,which can provide scientific basis for the basic research of the pharmacodynamic substances and the clinical safe use of the drug.
作者
岑芳
张霜
易蕾
伍国怡
黄健军
王若谷
王鑫
CEN Fang;ZHANG Shuang;YI Lei;WU Guoyi;HUANG Jianjun;WANG Ruogu;WANG Xin(Nanning Hospital of Traditional Chinese Medicine,Nanning 530000,China;Beihai Public Inspection and Testing Cen-ter,Beihai 536000,China;Guangxi University of Chinese Medicine,Nanning 530000,China)
出处
《特产研究》
2025年第2期135-143,共9页
Special Wild Economic Animal and Plant Research
基金
广西壮族自治区中医药管理局课题项目(GXZYA20230411)
广西中医药重点研究室建设项目(桂中医药科教发[2023]9号)
广西中医药大学科研项目(2022MS026)。
作者简介
岑芳(1982-),女,广西贺州人,硕士,副主任医师,从事中药治疗妇科疾病的研究;通讯作者:王若谷(1973-),男,硕士,高级工程师,从事质量管理及计量检测工作。
