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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 rapid screening and quantitative analysis method for the determination of 24 kinds of anti-inflammatory and analgesic compounds in proprietary Chinese medicines or health products by ultra performance liquid chromatography-quadrupole / electrostatic field orbit trap mass spectrometry. Methods The mobile phase was eluted with acetonitrile and 0.02 mol·L -1 ammonium acetate solution on a Thermo Hypersil Gold C18 column (2.1 mm × 100 mm, 1.9 μm) with a column temperature of 30 ° C and a flow rate of 0.3 m L · Min ~ (-1); electrospray ionization of positive and negative ions at the same time, two full-scale high-precision scanning to get the accurate precursor ion mass and accurate fragment ion information, at the same time qualitative and quantitative analysis. Results The detection limit of each component in this method was 10.0 ~ 45.0 pg, and the recoveries ranged from 79.6% to 98.3%. In 45 batches of samples, 30 batches of positive samples were detected, the positive rate was 66.7%. The detected components were acetaminophen, diclofenac sodium, indomethacin, ibuprofen and so on. Conclusion The method has the advantages of convenient operation, high accuracy, high sensitivity and high selectivity. It can be used in the qualitative screening and quantitative analysis of illegally added chemical components in anti-inflammatory and analgesic samples.