脑栓通胶囊高效液相色谱指纹图谱质量控制方法研究  

HPLC fingerprint for the quality control of Naoshuantong capsules

作　　者：陈思[1] 谢称石 刘忠政[1] 彭维[1] 苏薇薇[1] 

机构地区：[1]中山大学生命科学学院,广州510275 [2]广东众生药业股份有限公司,广东东莞523325

出　　处：《中南药学》2013年第6期457-461,共5页Central South Pharmacy

基　　金：国家科技支撑计划课题(No.2012BAI29B09);广东省教育部科技部产学研结合项目(No.2011A091000008)

摘　　要：目的建立脑栓通胶囊HPLC指纹图谱,用于脑栓通胶囊质量控制。方法分别构建脑栓通胶囊HPLC指纹图谱A和HPLC指纹图谱B,共同检出复方中的全部5味药材成分。采用2种样品前处理方法(超声提取、超声提取后液液萃取纯化)制备脑栓通胶囊供试品溶液,使用Ultimate AQ-C18(150 mm×4.6 mm,3μm)色谱柱进行色谱分离。指纹图谱A色谱条件如下:以乙腈(A)-四氢呋喃(B)-0.05%磷酸溶液(C)为流动相,检测波长在0～53 min为254 nm,于53 min后将波长切换为275 nm,柱温20℃,流速1.1 mL min-1;指纹图谱B色谱条件如下:以乙腈(A)-0.05%磷酸溶液(B)为流动相,检测波长390 nm,柱温25℃,流速1.0 mL min-1。结果脑栓通胶囊指纹图谱A(可检出蒲黄、赤芍、天麻、漏芦4味药材)确定了27个共有峰,通过对照品对照、快速液相-三重串联四级杆质谱(RRLC/MS/MS)鉴定了其中10个色谱峰的化学成分;脑栓通胶囊指纹图谱B(可检出郁金药材)确定了5个共有峰,鉴定了其中1个色谱峰的化学成分。结论该方法具有良好的可行性、稳定性和重现性,为脑栓通胶囊的质量控制提供了科学依据。Objective To develop the HPLC fingerprint of Naoshuantong capsules and control its quality.Methods HPLC fingerprint A and B of Naoshuantong capsules which displayed chromatographic peaks covering 5 medicinal materials were established.The samples were obtained by ultrasonic extraction and liquid-liquid extraction after ultrasonic method,and the chromatographic separation of 2 samples was performed on an Ultimate AQ-C18（150 mm×4.6 mm,3 μm） column.The HPLC fingerprint A was established with acetonitrile（A）-tetrahydrofuran（B）-0.05% phosphoric acid（C） as the mobile phase at 1.1 mL min-1.The detection wavelength was 254/275 nm,and column temperature was 20 ℃.The HPLC fingerprint B was obtained with acetonitrile（A）-0.05% phosphoric acid（B） as the mobile phase at 1.0 mL min-1.The detection wavelength and column temperature were set at 390 nm and 25 ℃.Results In the established fingerprint A,27 common chromatographic peaks covering Typhae Pollen,Paeoniae Radix Rubra,Gastrodiae Rhizoma and Rhapontici Radix were detected,and 10 chemical compounds were identified by comparing the reference substance with RRLC/MS/MS.In the established fingerprint B,5 common chromategraphic peaks covering Curcumae Radix were detected,but only 1 chemical compound was identified.Conclusion The method can be used for the quality control of Naoshuantong capsules with great precision and good reproducibility.

关 键 词：脑栓通胶囊 高效液相色谱法 指纹图谱 

分 类 号：O657.7[理学—分析化学]