摘要
目的:建立医院制剂克白合剂的HPLC对照指纹图谱,为科学评价和有效控制其质量提供可靠的方法,并对其可能存在的有害残留物进行检测。方法:采用HPLC法对克白合剂进行了多成分指纹图谱研究,对主要的色谱峰进行了归属性分析及相似度评价;采用原子吸收分光光度法对制剂中的铅、镉、砷、汞、铜等重金属及有害元素、采用气相色谱法对六六六等有机氯类农药残留量进行测定;采用平皿法对微生物等进行限度测定。结果:以S1样品(S1为方法学样品)图谱作为参照图谱,采用平均数法,时间窗宽度为0.1,经过多点校正后自动匹配,形成保留时间较为稳定、峰形明显的19个共有峰图谱作为样品对照指纹图谱,10批克白合剂样品与对照指纹图谱比较相似度均高于0.90;克白合剂中的铅、镉、砷、汞、铜等重金属及有害元素、六六六等有机氯类农药残留量及微生物均未超出《中国药典》2020年版的相关执行标准。结论:所建立的指纹图谱为复方制剂的全面质量控制探索一条可行之路,并为其临床用药的安全性与有效性提供质量保障。
Objective:To establish HPLC fingerprints of Kebai Mixture,provide a reliable evaluation method for scientific evaluation and effective quality control of Kebai Mixture,and to detect the harmful residue substances in Kebai Mixture.Methods:The multi-component fingerprints of Kebai Mixture were studied by an HPLC method,and the main chromatographic peaks were analyzed by attribution analysis and similarity evaluation.The atomic absorption spectrophotometry(AAS)was used to determine the contents of heavy metals such as lead,cadmium,arsenic,mercury,copper.Gas chromatography was used to determine the residues of organochlorine pesticides.The limit of microorganism was measured by a plate method.Results:The S1 sample(the methodological sample)chromatograms were used as the reference,a mean method was adopted,the time window width was 0.1,19 common peaks with stable retention time and obvious peak shape were automatically matched after multi-point correction.The comparison similarity between 10 batches of Kebai Mixture samples and the control fingerprints was higher than 0.90.The residues of heavy metals such as lead,cadmium,arsenic,mercury and copper and harmful elements such as organochlorine pesticides and microorganisms in Kebai Mixture did not exceed the relevant implementation standards of Chinese Pharmacopoeia in the 2020 edition.Conclusion:The established fingerprint method can explore a feasible way for the comprehensive quality control of compound preparations,and provide quality guarantee for the safety and effectiveness of clinical medication.
作者
童菊华
黄巧玲
王迅
吴经耀
徐强
TONG Juhua;HUANG Qiaoling;WANG Xun;WU Jingyao;XU Qiang(Zhejiang Research Institute of Traditional Chinese Medicine,Hangzhou 310023,China;Department of Pharmacy,the Third People's Hospital of Hangzhou,Hangzhou 310009,China)
出处
《药学与临床研究》
2022年第3期225-228,232,共5页
Pharmaceutical and Clinical Research
基金
浙江省中医药科学研究基金项目(2016ZA167)。
关键词
克白合剂
质量评价
指纹图谱
有害残留物质
Kebai mixture
Quality evaluation
Fingerprint
Harmful residue substances
