菥蓂配方颗粒特征图谱及含量测定研究  

Characteristic Chromatograms and Content Determination of Thlaspi Herba Formula Granules

作　　者：李英哲 李佳东 黄梦龙 周明哲 吴弢[1] LI Yingzhe;LI Jiadong;HUANG Menglong;ZHOU Mingzhe;WU Tao(Institute of Chinese Materia Medicine,Shanghai University of Chinese Medicine,Shanghai,China 201203)

机构地区：[1]上海中医药大学中药研究所,上海201203

出　　处：《中国药业》2023年第6期60-66,共7页China Pharmaceuticals

摘　　要：目的 建立菥蓂配方颗粒的超高效液相色谱(UPLC)特征图谱和含量测定方法。方法 采用超高效液相色谱串联质谱(UPLCMS/MS)法表征菥蓂药材主要化合物。色谱柱为Agilent InfinityLab Poroshell 120 SB-C18柱(100 mm×4.6 mm,2.7μm),流动相为乙腈-0.1%甲酸溶液(梯度洗脱),流速为0.8 mL/min,检测波长为336 nm,柱温为30℃,进样量为10μL;以异牡荆素峰为参照峰,测定12批颗粒样品、1批饮片样品的UPLC特征图谱,采用中药色谱特征图谱相似度评价系统(2012版)进行相似度评价。测定异牡荆素的含量。结果 共表征14个化合物,其中10个化合物(柠檬酸、丹参素、原儿茶酸、异荭草苷、荭草苷、异牡荆素、当药黄素、大波斯菊苷、木犀草素、芹菜素)经对照品验证,柠檬酸、丹参素、原儿茶酸及荭草苷4个化合物为首次从菥蓂药材中检出。建立以异牡荆素、异肥皂草苷、异荭草苷、木犀草素为特征峰的UPLC指纹图谱,10批颗粒样品(均来自同一公司)相似度为0.998~1.000。异牡荆素质量浓度在2.54~254.00μg/mL范围内与峰面积积分值线性关系良好(R^(2)=0.999 6);精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率为99.62%,RSD小于3%(n=9)。结论 该UPLC特征图谱和含量测定方法稳定准确,可为菥蓂配方颗粒的评价及质量控制提供参考。ObjectiveTo establish ultra-high performance liquid chromatography(UPLC) characteristic chromatograms and content determination method for Thlaspi Herba Formula Granules.MethodsThe main compounds of Thlaspi Herba were characterized by UPLC-mass spectrometry(UPLC-MS/MS).The chromatographic column was Agilent InfinityLab Poroshell 120 SB-C18column(100 mm × 4.6 mm,2.7 μm),the mobile phase was acetonitrile-0.1% formic acid solution(gradient elution),the flow rate was 0.8 mL/min,the detection wavelength was 336 nm,the column temperature was 30 ℃,and the injection volume was 10 μL.With the isovitexin peak as the reference peak,the UPLC characteristic chromatograms of twelve batches of granule samples and one batch of decoction pieces were determined,and the Similarity Evaluation System for the Chromatographic Fingerprint of Traditional Chinese Medicine(Version 2012) was used for similarity evaluation.The content of isovitexin was determined.ResultsA total of14 compounds were characterized,of which 10 compounds(citric acid,salvianic acid A,protocatechuic acid,isoorientin,orientin,isovitexin,swertisin,apigenin-7-O-glucoside,luteolin,and apigenin) were confirmed by the reference substances.Citric acid,salvianic acid A,protocatechuic acid,and orientin were reported for the first time from Thlaspi Herba.The UPLC fingerprints with isovitexin,isosaponin,isoorientin and luteolin as the characteristic peaks were established.The similarity of 10 batches of granule samples(all from the same company) was in the range of 0.998-1.000.The linear range of isovitexin was 2.54-254.00 μg/mL(R^(2)= 0.999 6).The RSDs of precision,stability and repeatability tests were less than 2.0%.The average recovery of isovitexin was99.62%,and its RSD was less than 3%(n = 9).ConclusionThe UPLC characteristic chromatograms and content determination method are stable and accurate,which can provide a reference for the evaluation and quality control of the Thlaspi Herba Formula Granules.

关 键 词：菥蓂 配方颗粒 超高效液相色谱串联质谱法 特征图谱 异牡荆素 含量测定 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]