HPLC-PDA-MS/MS法研究热毒宁注射液生产过程中栀子化学成分的变化  

Research on constituent change of Gardenia jasminoides Ellis during production process of Reduning injection by HPLC-PDA-MS/MS

作　　者：朱强[1] 王艳娟[1,2] 王振中[2] 萧伟[2] 李发美[1] 熊志立[1] 

机构地区：[1]沈阳药科大学药学院,辽宁沈阳110016 [2]江苏康缘药业股份有限公司,江苏连云港222001

出　　处：《沈阳药科大学学报》2013年第6期429-438,共10页Journal of Shenyang Pharmaceutical University

摘　　要：目的采用高效液相色谱光电二极管阵列检测器串联质谱技术(HPLC-PDA-MS/MS)定性研究栀子药材、栀子中间体以及热毒宁注射液的化学成分。方法采用Agilent Eclipse XDB-C18柱(4.6mm×250 mm,5μm),以乙腈体积分数0.3%乙酸水溶液为流动相进行梯度洗脱,流速1.0 mL.min-1;质谱采用ESI源,正负离子同时检测,在m/z 150～800内进行扫描,并对特征离子进行二次裂解,获得二级质谱数据。结果栀子药材共检测到20种化学成分,与对照品对比,确定了栀子苷等10种化学成分;通过紫外光谱信息、一级和二级质谱数据,推测出去乙酰基车前草酸等8种化学成分。其中京尼平酸、京尼平龙胆双糖苷、栀子苷、绿原酸、新绿原酸、隐绿原酸、异绿原酸A、异绿原酸B、异绿原酸C以及一未知成分共10种化学成分在热毒宁注射液生产过程中从栀子药材经栀子中间体转移至热毒宁注射液中。结论利用HPLC-PDA-MS/MS对热毒宁注射液生产过程中药材栀子化学成分变化情况进行了研究,为热毒宁注射液生产过程质量控制与评价提供依据。Objective To analyze chemical constituents of Gardenia jasminoides Ellis,intermediate of Gardenia jasminoides Ellis and Reduning injection using high-performance liquid chromatography coupled with photo-diode-array detector and tandem mass spetrometry（HPLC-PDA-MS/MS）.Methods Agilent Eclipse XDB-C18 column（4.6 mm×250 mm,5 μm）was adopted,with gradient elution system of water containing 0.3% acetic acid and acetonitrile at flow rate of 1.0 mL · min-1.The mass spectra were obtained by electrospray ionization source operating in both positive and negative ion mode.Ions were scanned from the m/z 150 to 800,and the characteristic ions were schizolysised twice to obtain the secondary MS data.Results Twenty chemical constituents were detected in Gardenia jasminoides Ellis.Ten chemical constituents including geniposide were compared with reference standards.Eight chemical constituents were identified by comparing UV spectra,the MS and MS2 data with the related literature,such as deacetylasperulosidic acid.It was found that ten chemical constituents including geniposidic acid,genipin-1-D-gentiobioside,geniposide,chlorogenic acid,neochlorogenic acid,cryptochlorogenic acid,isochlorogenic acid A,isochlorogenic acid B,isochlorogenic acid C and an unkown constituent were transferred to Reduning injection through intermediate of Gardenia jasminoides Ellis.Conclusions The change of constituent from Gardenia jasminoides Ellis during the production process of Reduning injection is analyzed by HPLC-PDA-MS/MS and provide a basis for Reduning injection quality control during production process.

关 键 词：液质联用 热毒宁注射液 栀子 生产过程 化学成分 

分 类 号：R914[医药卫生—药物化学] R917[医药卫生—药学]