液相色谱-质谱联用法同时测定岩白菜中熊果苷等9种成分的含量  

Simultaneous Determination of Nine Compounds in Bergenia purpurascens by HPLC-MS

作　　者：任艳平[1] 曹亮[1] 常路[1] 支旭然[1] 苑霖[1] 生宁[1] 张兰桐[1] 

机构地区：[1]河北医科大学药学院药物分析教研室,石家庄050017

出　　处：《中国药学杂志》2013年第6期477-481,共5页Chinese Pharmaceutical Journal

摘　　要：目的采用HPLC-MS测定岩白菜中熊果苷、没食子酸、岩白菜素、原儿茶酸、绿原酸、儿茶素、表儿茶素、表儿茶素没食子酸酯和阿魏酸9种成分的含量。方法采用Diamonsil C18柱(4.6 mm×150 mm,5μm);柱温为室温;流动相为甲醇体积分数为-0.2‰甲酸水,以0.8 mL·min-1的流速进行梯度洗脱,进样量10μL;质谱条件:采用电喷雾离子源进行负离子模式检测,多反应监测模式(MRM)用于定量测定。结果岩白菜中9种成分熊果苷、没食子酸、岩白菜素、原儿茶酸、绿原酸、儿茶素、表儿茶素、表儿茶素没食子酸酯和阿魏酸能完全分离;峰面积与浓度呈良好的线性关系。平均回收率(n=9)分别为100.2%,100.0%,99.8%,99.9%,97.9%,101.2%,99.8%,101.7%,102.4%。RSD分别为0.80%,3.06%,2.72%,3.28%,3.58%,1.44%,0.95%,0.96%,0.48%。结论该方法简便,准确,重现性好,专属性高,可用于岩白菜中多种成分的含量测定和质量控制。OBJECTIVE To develop a method for the determination of arbutin, gallic acid, bergenin, protocatechuic acid, chlo- rogenic acid, catechin, epicatechin, epicatechin gallate, and ferulic acid in Bergenia purpurascens by HPLC-MS/MS. METHODS The samples were separated on a Diamonsil C18 column （4.6 mm×150mm,5μm） by gradient elution using methanol and 0. 2%v （V/V） formic acid aqueous solution as the mobile phase at a flow rate of 0. 8 mL ·min^-1 The column temperature was room temperature. Multiple-reaction monitoring （MRM） scanning was employed for quantification with switching electrospray ion source polarity in negative mode. RESULTS Complete separation was achieved within 10 rain for the nine compounds （arbutin, gallic acid, bergenin, protoeatechuic acid, chlorogenic acid, catechin, epieatechin, epicatechin gallate, ferulic acid）. The nine regression equations showed linear relationships between peak areas and contents of each compound. The average recoveries （ n = 9 ） of the compounds listed above were 100.2%, 100.0%, 99.8%, 99.9%, 97.9%, 101.2%, 99.8%, 101.7%, 102. 4% and RSD were 0.80%, 3.06%, 2. 72% , 3.28% , 3.58% , 1.44% , 0. 95% , 0. 96% , 0.48% , respectively. CONCLUSION The method is simple, accurate and has good reproducibility, thus can be used for the determination of the nine compounds in Bergenia purpurascens.

关 键 词：高效液相色谱-质谱联用法 岩白菜 熊果苷 岩白菜素 含量测定 

分 类 号：R917[医药卫生—药物分析学]