多中心切割二维液相色谱法同时测定九味熄风颗粒中10种成分  

Simultaneous quantitation of 10 components in Jiuwei Xifeng Granules by multiple heart-cutting two dimensional liquid chromatography

作　　者：沈灿杰 马阳[1,2] 陈夏霖 高霞[1,2] 曹亮[1,2] 王振中[1,2] 肖伟[1,2] SHEN Can-jie;MA Yang;CHEN Xia-Lin;GAO Xia;CAO Liang;WANG Zhen-zhong;XIAO Wei(Jiangsu Kanion Pharmaceutical Co.,Ltd.,Lianyungang 222001,China;State Key Laboratory of New-Tech for Chinese Medicine Pharmaceutical Process,Lianyungang 222001,China;China Pharmaceutical University,Nanjing 211198,China)

机构地区：[1]江苏康缘药业股份有限公司,江苏连云港222001 [2]中药制药过程新技术国家重点实验室,江苏连云港222001 [3]中国药科大学,江苏南京211198

出　　处：《中草药》2022年第14期4333-4339,共7页Chinese Traditional and Herbal Drugs

基　　金：江苏省工信厅2020年度工业和信息产业转型升级专项资金项目-多组分中药研究关键技术。

摘　　要：目的采用在线多中心切割二维液相色谱法,建立同时测定九味熄风颗粒中10种成分的含量测定方法。方法第一维采用Acquity BEH C18(100 mm×3.0 mm,1.7μm)为色谱柱,第二维色谱柱为X Select HSS T3(250 mm×4.6 mm,5μm);流动相均采用甲醇-乙腈(95∶5)混合溶液-磷酸水体系,梯度洗脱;体积流量分别为0.2、1.0 mL/min;柱温35℃。结果同时测定了九味熄风颗粒中次黄嘌呤、天麻素、有机酸类(原儿茶酸、新绿原酸、绿原酸、隐绿原酸)、环烯醚萜苷类(马钱苷酸、獐芽菜苦苷、龙胆苦苷、当药苷)10种成分的含量,各成分在考察的质量浓度范围内线性关系良好(r≥0.999),精密度RSD均小于2%,重复性RSD均小于5%,供试品溶液室温24 h内稳定,平均加样回收率为97.45%~104.82%,13批制剂中次黄嘌呤、天麻素、原儿茶酸、新绿原酸、绿原酸、马钱苷酸、隐绿原酸、獐芽菜苦苷、龙胆苦苷、当药苷质量分数分别为0.034~0.111、1.224~2.078、0.032~0.055、0.010~0.066、0.202~0.341、1.052~1.542、0.016~0.080、0.151~0.333、4.560~7.354、0.343~0.518mg/g,其中天麻素、总有机酸、总环烯醚萜苷类成分的批间一致性良好。结论建立的方法操作简便,结果准确、可靠,可用于九味熄风颗粒的质量控制和评价。Objective To develop an online multiple heart-cutting two-dimensional liquid chromatography method for the simultaneous determination of 10 components from the Jiuwei Xifeng Granules(JXG).Methods The first dimensional column was Acquity UPLC BEH C18(100 mm×3.0 mm,1.7μm)and the second dimensional column was X Select HSS T3(250 mm×4.6 mm,5μm).The mobile phase was methanol-acetonitrile mixed solution(95:5)and phosphoric acid-water solution.The flow rates were 0.2 mL/min and 1.0 mL/min respectively in two dimensions.And column temperature controled at 35℃.Results The contents of hypoxanthine,gastrodin,organic acids(protocatechuic acid,neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid)and iridoid glycosides(loganic acid,swertiamarine,gentiopicroside,sweroside)in JXG were determined simultaneously.Each component had a good linear relationship within the investigated concentration range(r≥0.999),the RSD of precision were less than 2%,the RSD of repeatability were less than 5%,and the sample solution was stable within 24 h at room temperature,the average recovery were 97.45%—104.82%,and the consistency of 13 batches of test samples are good.The concentration of hypoxanthine,gastrodin,protocatechuic acid,neochlorogenic acid,chlorogenic acid,loganic acid,cryptochlorogenic acid,swertiamarine,gentiopicroside,sweroside in 13 batches of samples were 0.034—0.111,1.224—2.078,0.032—0.055,0.010—0.066,0.202—0.341,1.052—1.542,0.016—0.080,0.151—0.333,4.560—7.354,0.341—0.638 mg/g,respectively,and the consistency of gastrodin,total organic acid and total iridoid glycosides were good.Conclusion The estabilshed method is simple,accurate and reliable,which can be used for the quality control and evaluation of JXG.

关 键 词：九味熄风颗粒 二维液相色谱 中心切割 同时测定 次黄嘌呤 天麻素 有机酸类 原儿茶酸 新绿原酸 绿原酸 隐绿原酸 环烯醚萜苷类 马钱苷酸 獐芽菜苦苷 龙胆苦苷 当药苷 质量控制 

分 类 号：R286.02[医药卫生—中药学]