基于UFLC-Triple TOF-MS/MS技术的枳实传统饮片及破壁饮片化学成分系统分析  

Chemical constituents in traditional slices and ultrafine granular powder of Fructus Aurantii Immaturus by UFLC-Triple TOF-MS/MS

作　　者：郑玉莹 庞文静 白杨[1,2] 邓雯 成金乐 吴忠 彭维 苏薇薇[1,2] ZHENG Yu-ying;PANG Wen-jing;BAI Yang;DENG Wen;CHENG Jin-le;WU Zhong;PENG Wei;SU Wei-wei(School of Life Sciences, Sun Yat-sen University, Guangzhou 510275;Guangdong Engineering ＆ Technology Research Center for Quality and Efficacy Reevaluation of Post-Market Traditional Chinese Medicine, Guangzhou 510275;ZEUS Pharmaceutical Group, Zhongshan Guangdong 528437)

机构地区：[1]中山大学生命科学学院,广州510275 [2]广东省中药上市后质量与药效再评价工程技术研究中心,广州510275 [3]中山市中智药业集团有限公司,广州中山528437

出　　处：《中南药学》2018年第4期443-450,共8页Central South Pharmacy

基　　金：广东省中医药局科研项目(No.20161050)

摘　　要：目的基于超快速高效液相色谱串联四极杆飞行时间质谱技术(UFLC-Triple Q-TOF-MS/MS),对同批次的枳实传统饮片和破壁饮片的整体化学成分进行鉴定分析,探讨破壁粉碎技术对饮片化学成分的影响。方法采用Phenomenex C18色谱柱(3.0 mm×150 mm,2.6μm),以乙腈和0.1%甲酸溶液为流动相梯度洗脱,流速0.3 m L·min-1;采用ESI电喷雾源的高分辨三重四极杆飞行时间质谱,分别在正、负离子模式下进行检测。结果根据正负离子模式下获得的一级和二级质谱数据,通过准确分子量、裂解碎片及文献,共确证和指证出54个化合物,其中32个黄酮类成分,14个香豆素类成分,3个生物碱类成分,2个挥发油类成分,2个柠檬苦素类成分和1个有机酸类成分。结论枳实传统饮片经破壁工艺加工后,化学成分种类无差异。本研究可为枳实传统饮片与破壁饮片的进一步研究及质量控制提供科学依据。Objective To systematically identify the chemical constituents and compare the differences between traditional slices and ultrafine granular powder of Fructus Aurantii lmmaturus by UFLC-Triple TOF-MS/MS. Methods Phenomenex C18 column （3.0 mm × 150 mm, 2.6 μm） was used with acetonitrile and 0.1% formic acid solution as the mobile phase in gradient elution. The flow rate was 0.3 mL ·main-1. The detector was high-resolution quadrupole time of flight mass spectrometry with ESI ion source, tested in both positive and negative models. Results Based on the analysis of mass spectrometry and certification of reference substances, 54 compounds were confirmed, including 32 flavonoids, 3 alkaloids, 14 cournarins, 2 volatile oils, 2 limonin and 1 organic acid ingredient. Conclusion There is no difference in the chemical composition types after a superfine grinding process of Fructus durantii lmmaturus. The study has provided scientific basis for further research and quality control of traditional decoction of traditional slices and ultrafine granular powder of Fructus Aurantii lmmaturus.

关 键 词：枳实 传统饮片 破壁饮片 三重四极杆飞行时间质谱 化学成分 

分 类 号：R284.1[医药卫生—中药学] O657.63[医药卫生—中医学]