中国中药杂志

2013, v.38(20) 3502-3506

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生血宁片指纹图谱的研究
Study on fingerprint of Shengxuening tablets

聂晶;胡华胜;陈晓颙;刘娟娟;李珂;罗京;
NIE Jing;HU Hua-sheng;CHEN Xiao-yong;LIU Juan-juan;LI Ke;LUO Jing;Hubei Institute for Food and Drug Control;College of Pharmaceutical Sciences,Hubei Chinese Medical University;Tongji Medical College of Huazhong University of Science & Technology;Wuhan United Pharmaceutical Co. ,Ltd.;

摘要(Abstract):

建立中药制剂生血宁片指纹图谱研究方法。以二氢卟吩e6(chlorin e6)为对照品,采用SHISEIDO Capcell-pak C18色谱柱(4.6 mm×250 mm,5μm),以0.2%甲酸溶液[含20 mmol·L-1四丁基溴化铵(TBAB)]为流动相A,乙腈-甲醇-丙酮(50∶50∶5)为流动相B,梯度洗脱,检测波长392 nm,流速1.0 mL·min-1,柱温45℃。指纹图谱共标定10个共有峰,各共有峰相对保留值变化的RSD均在0.50%之内,采用UPLC/DAD/Q-TOF-MS xevo G2 Q-Tof LC/MS初步归属了其中6个色谱峰。生血宁片中主要含叶绿素的铁代衍生物,主要成分是铁二氢卟吩p6,铁二氢卟吩e6,铁异二氢卟吩e4等。
To establish a method for studying fingerprint of Shengxuening tablets. With chlorin e6 as the reference substance, SHISEIDO Capcell-pak C 18( 4. 6 mm ×250 mm,5 μm) analytical column was adopted and eluted with 0. 2% formic acid( containing 20 mmol·L- 1TBAB)( A) and acetonitrile-methanol-acetone( 50∶ 50∶ 5)( B). The detection wavelength was set 392 nm. The volume flow rate was 1. 0 mL·min- 1. The temperature of column was 45 ℃. Totally 10 common peaks were indicated on the HPLC fingerprint,with RSDs for variable retention values in common peaks below 0. 50%. UPLC/DAD/Q-TOF-MS xevo G2 Q-TOF LC/MS was adopted to preliminarily indentify six chromatographic peaks. The main ingredient in Shengxuening tablets was ferrous derivative,which was mainly composed of Fe chlorin p6,Fe chlorin e6 and Fe isochlorin e4.

关键词(KeyWords): 生血宁片;指纹图谱;UPLC/DAD/Q-TOF-MS
Shengxuening tablets;fingerprint;UPLC/DAD/Q-TOF-MS

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作者(Author): 聂晶;胡华胜;陈晓颙;刘娟娟;李珂;罗京;
NIE Jing;HU Hua-sheng;CHEN Xiao-yong;LIU Juan-juan;LI Ke;LUO Jing;Hubei Institute for Food and Drug Control;College of Pharmaceutical Sciences,Hubei Chinese Medical University;Tongji Medical College of Huazhong University of Science & Technology;Wuhan United Pharmaceutical Co. ,Ltd.;

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