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[摘要]
目的 建立疏风解毒胶囊(SJC)HPLC指纹图谱分析方法,为全面有效控制其质量提供依据。方法 采用HPLC法建立SJC指纹图谱,色谱条件:Unitary C18色谱柱(250 mm×4.6 mm,5 μm),以乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,体积流量1.0 mL/min,柱温30 ℃,检测波长250 nm,进样量10 μL;对所建指纹图谱进行相似度分析及主成分分析(PCA),并对共有峰进行药材归属及成分指认。结果 建立了SJC HPLC指纹图谱共有模式,确定了22个共有峰;14批SJC相似度在0.915~0.977,PCA表明前3个主成分代表了原始HPLC指纹图谱的主要信息;在指纹图谱所标定的22个共有峰中,8、12、13、14、15、16、21、22号峰来自虎杖,1、2、3、7、9、10号峰来自连翘,5、6、11号峰来自马鞭草,4号峰来自败酱草,18、19号峰来自甘草,17、20号峰未能归属到具体药材;通过质谱数据比对,共指认出16个共有峰,分别为1号峰(连翘酯苷E)、5号峰(戟叶马鞭草苷)、6号峰(马鞭草苷)、7号峰(5'-羟基连翘酯苷A)、8号峰(虎杖苷)、9号峰(连翘苷)、10号峰(连翘酯苷A)、11号峰(毛蕊花糖苷)、12号峰(异连翘酯苷A)、13号峰(芦荟大黄素)、14号峰(大黄素-8-O-葡萄糖苷)、15号峰(大黄酸)、18号峰(甘草酸单铵盐)、19号峰(3-羟基光甘草酚)、21号峰(大黄素)、22号峰(大黄酚)。结论 首次建立了SJC HPLC指纹图谱分析方法,该法操作简单、准确,精密度、重复性好,可较全面地反映SJC中化学成分的信息,为SJC质量控制提供了可靠的科学依据。
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[Abstract]
Objective To establish an HPLC method for the fingerprint analysis of ShufengJiedu Capsule (SJC), so as to provide evidence for the quality control of it. Methods HPLC method was applied with the chromatographic condition as follows: The chromatographic column was Unitary C18 column (200 mm × 4.6 mm, 5 μm), acetonitrile-0.1% formic acid as the mobile phase with gradient elution, the flow rate was 1.0 mL/min, the detection wavelength was 250 nm, the column temperature was 30 ℃, and the injection volume was 10 μL. The HPLC fingerprint of SJC was analyzed with similarity analysis and principal component analysis (PCA) method. ResultsThe fingerprint chromatography included 22 mutual peaks, of which eight mutual peaks fromPolygonumcuspidatum, six mutual peaks from Forsythia suspensa, three mutual peaks from Verbena officinalis, two mutual peaks from Glycyrrhizauralensis, and one mutual peak fromThlaspiarvense. The similarity among 14 batches was more than0.9. Based on the HPLC-MS2 data, 16 components were identified, which were forsythosid E, hastatoside, verbenalin,5'-hydroxy-forsythiasideA,polydatin, phillyrin, forsythosid A, acteoside, iso-forsythosid A, aloe-emodin, emodin-8-O-grapeglycosides, parieticacid, monoammoniumglycyrrhizinate, 3-hydroxyglabrol, emodin, and chrysophanol. Conclusion It is the first time to establish the HPLC fingerprint of SJC. The method is simple, accurate, and reproducible, which could reflect the chemical composition information of SJC comprehensively and provide scientific evidence for the quality control.
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