基于UPLC指纹图谱结合化学计量学方法评价癃闭舒制剂  

Quality Evaluation of Longbishu Preparations Based on UPLC FingerprintCombined with Chemometric Methods

作　　者：申莉萍 王嘉伟 胡晓[1] 靳建杰 黄春跃[1] SHEN Liping;WANG Jiawei;HU Xiao;JIN Jianjie;HUANG Chunyue(State Key Lab.of New Drug and Pharmaceutical Process,Shanghai Institute of Pharmaceutical Industry Co.,Ltd.,China State Institute of Pharmaceutical Industry,Shanghai 201203)

机构地区：[1]中国医药工业研究总院上海医药工业研究院有限公司,创新药物与制药工艺国家重点实验室,上海201203

出　　处：《中国医药工业杂志》2022年第9期1298-1305,共8页Chinese Journal of Pharmaceuticals

基　　金：国家自然科学基金(81803844,81402824);上海市自然科学基金(19ZR1454400,21ZR1461800);中央引导地方科技发展资金(GZIM 202001-9-2)。

摘　　要：建立了癃闭舒(1)制剂的超高效液相色谱(UPLC)指纹图谱。采用UPLC技术对1制剂的甲醇提取液进行分析,色谱柱采用Waters ACQUITY UPLC^(■)HSS T_(3)柱(2.1 mm×100 mm,1.8μm),流动相A为0.1%磷酸溶液,B为乙腈,梯度洗脱。流速为0.2 ml/min,柱温为30℃,检测波长为221 nm。采用中药色谱指纹图谱相似度评价系统确定12个色谱峰作为1胶囊对照指纹图谱的共有峰,并通过与标准品比对,指认了9个共有峰。采用相似度分析、主成分分析及正交偏最小二乘法分析等化学计量学方法,对39批不同厂家的1胶囊及片剂进行分析。结果显示1胶囊和1片具有一定的差异性,其中5个共有峰(峰1、8、9、10和11)的差异性显著,反映出不同厂家1制剂生产所用的补骨脂和山慈菇药材质量各异。建立的方法简便、快速、准确且可重复,为1制剂的质量评价提供了试验依据。The ultra-high performance liquid chromatography(UPLC)fingerprints of Longbishu(1)preparations were established.The methanol extract of 1 preparation was analyzed by UPLC.The Waters ACQUITY UPLC^(■)HSS T_(3)_ column(2.1 mm×100 mm,1.8μm)was used,and the analysis was carried out in the gradient elution mode with 0.1%phosphoric acid solution as mobile phase A,and acetonitrile as mobile phase B.The flow rate was 0.2 ml/min,the column temperature was 30℃,and the detection wavelength was 221 nm.Twelve chromatographic peaks were identified as the common peaks of the control fingerprints of 1 capsules by the Chinese medicine chromatographic fingerprint similarity evaluation system,and nine common peaks were identified by comparing with the standard.Chemometric methods such as similarity analysis,principal component analysis and orthogonal partial least squares analysis were used to analyze thirty-nine batches of 1 capsules and tablets from different manufacturers.The results showed that there were certain differences between 1 capsules and 1 tablets.Among them,five common peaks(peaks 1,8,9,10 and 11)were significantly different,reflecting the differences in the quality of malaytea scurfpea fruit and appendiculate cremastra pseudobulb used by different manufacturers when producing 1 preparations.The established method is simple,rapid,accurate and reproducible,which provides an experimental basis for the quality evaluation of 1 preparations.

关 键 词：癃闭舒胶囊 癃闭舒片 超高效液相色谱 质量评价 指纹图谱 化学计量法 

分 类 号：R917[医药卫生—药物分析学]