基于特征离子的血竭和龙血竭UPLC-QTOF/MS定性鉴别方法的建立  

Identification of Draconis Sanguis and Resina Draconis based on characteristic ions by UPLC- QTOF / MS

作　　者：刘薇[1] 李明华[1] 陆以云 程显隆[1] 魏锋[1] 马双成[1] 

机构地区：[1]中国食品药品检定研究院,北京100050

出　　处：《药物分析杂志》2015年第10期1777-1781,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：重大新药创制"中药安全检测技术及标准平台"(2014ZX09304307-002)

摘　　要：目的：寻找血竭和龙血竭药材的专属性成分,形成以特征离子为目标的鉴别方法。方法：利用超高效液相色谱-四极杆飞行时间-质谱（UPLC-QTOF/MS）进行测定,采用Markerlynx软件对血竭和龙血竭药材的质谱数据进行主成分分析,找出对区分药材有贡献的色谱峰,并采用软件对差异性成分进行鉴定。LC-MS条件：采用ACQUITY UPLC BEH C18（2.1 mm×100 mm,1.7μm）色谱柱,以0.1%甲酸水溶液（A）-乙腈（B）为流动相,梯度洗脱（0～10 min,5%B→95%B;10～11 min,95%B;11～11.1 min,95%B→5%B;11.1～15 min,5%B）,流速0.25 m L·min-1,柱温40℃;质谱采用离子化模式为ESI＋,毛细管电压3.0 k V,锥孔电压35 V,离子源温度105℃,扫描范围m/z 50～1 500。结果：根据主成分分析,血竭和龙血竭分别聚在不同的区域,显示血竭和龙血竭的化学成分有差异,可作为血竭和龙血竭的定性鉴别方法。结论：建立的方法可以用于区分血竭和龙血竭的定性鉴别。Objective： To search specific components and establish method for the identification of Draconis Sanguts and Resina Draconis based on characteristic ions. Methods： The sample was analyzed on a UPLC coupled with QTOF mass spectrometry. The UPLC- MS data of samples were subjected to principal component analysis（ PCA） in order to find the marker constituents. LC- MS conditions were as follows. The chromatographic column was ACQUITY UPLC BEH C18column（ 2. 1 mm × 100 mm,1. 7 μm）,the mobile phase was composed of 0. 1% formic acid（ A）and acetonitrile（ B） with gradient elution（ 0- 10 min,5% B→95% B; 10- 11 min,95% B; 11- 11. 1 min,95% B→5% B; 11. 1- 15 min,5% B）,the flow rate was 0. 25 m L·min- 1,and the column temperature was 40 ℃; the ionization mode was ESI＋,the capillary voltage was 3. 0 k V,the cone voltage was 35 V,and the ion source temperature was set at 105 ℃ at a scanning range of m / z 50- 1 500. Results： According to the results of PCA,Draconis Sanguts and Resina Draconis clustered in different regions and characteristic ions were found by OPLS. method for the identification of Draconis Sanguts and Resina Draconis based on characteristic ions was established. Conclusion： This method can be used for the identification of Draconis Sanguts and Resina Draconis.

关 键 词：超高效液相色谱-飞行时间质谱质谱 血竭 龙血竭 中药材鉴别 主成分分析(PCA) 

分 类 号：R917[医药卫生—药物分析学]