超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查及定量分析中成药或保健品中非法添加的24种消炎止痛类化学成分  

Rapid Screening and Quantitative Detection of 24 Illegally Added Anti-inflammatory Painkillers in Traditional Chinese Medicines and Health Foods by Ultra Performance Liquid Chromatography-Quadrupole /Electrostaticfield Orbitrap High Resolution Mass Spectro

作　　者：巩丽萍 田晨颖 郭常川 石峰 李军 姜树银 赵艳霞 

机构地区：[1]山东省食品药品检验研究院,济南250101 [2]山东中医药大学,济南250355

出　　处：《中国药学杂志》2015年第24期2154-2159,共6页Chinese Pharmaceutical Journal

基　　金：科技部国家重大科学仪器设备开发专项项目(2012YQ180132)

摘　　要：目的采用超高效液相色谱-四极杆/静电场轨道阱质谱建立中成药或保健品中24种消炎止痛类化学成分测定的快速筛查和定量分析方法。方法采用Thermo Hypersil Gold C18柱(2.1 mm×100 mm,1.9μm),以乙腈和0.02 mol·L^(-1)醋酸铵溶液为流动相,梯度洗脱,柱温30℃,流速0.3 m L·min^(-1);电喷雾电离正负离子同时一级、二级高精度全扫描,得到准确母离子质量数和准确碎片离子信息,同时进行定性定量分析。结果该方法中各成分的检出限为10.0~45.0 pg,回收率在79.6%~98.3%。45批样品中检出阳性样品30批,阳性率为66.7%,检出成分为对乙酰氨基酚、双氯芬酸钠、吲哚美辛、布洛芬等。结论该法具有操作方便、准确率高、灵敏度高、选择性高等优点,可用于消炎止痛类样品中非法添加化学成分的定性筛查和定量分析。OBJECTIVE To establish a method for rapid screening and quantification of 24 anti-inflammatory painkillers illegally added in traditional Chinese medicines and health foods by UPLC-quadrupole / electrostaticfield orbitrap high resolution mass spectrometry. METHODS The separation was performed on a Thermo Acquity UPLC system with a Hypersil Gold C18 column with gradient elution of acetonitrile and 20 mmol·L^-1 ammonium acetate solution. Electrospray ionization of positive and negative ions and one and two high precision full scan were used for the MS detection. The qualitative and quantitative analyses were carried out by accurate and precise parent ion mass and product ion mass information. RESULTS The limits of detection（ S / N ≥3） were 10. 0- 45. 0 μg ·kg^（-1）. The average recoveries were 79. 6%- 98. 3%. Thirty positive samples were detected among a total of 45 samples,resulting a positive rate of 66. 7%. The detected components were paracetamol,diclofenac sodium,indometacin,and ibuprofen. CONCLUSION The method is simple,highly accurate,sensitive and selective,and can be used in rapid screening and quantitative analysis of illegally added anti-inflammatory painkillers in traditional Chinese medicines and health foods.

关 键 词：超高效液相色谱 四极杆/静电场轨道阱高分辨质谱 消炎止痛 

分 类 号：R917[医药卫生—药物分析学]