目的:建立二维液相色谱-质谱联用法(2D-LC-MS/MS)测定中成药及保健品中4种抗痛风类药物成分含量的方法。方法:一维色谱柱:Agilent Zorbax SB-C18(4。6 mm × 50 mm，5 μm)，二维色谱柱:Agilent Poroshell 120 EC-C18(2。1 mm × 100 mm，2。7 μm)，流动相A:0。1％甲酸溶液(含5 mmol·L-1甲酸铵)，流动相B:乙腈，梯度洗脱，柱温:40℃，进样量:2 μL，电喷雾离子源，正离子检测模式，多反应监测模式。结果:萘丁美酮、酮咯酸氨丁三醇、倍他米松、地塞米松在各自浓度范围内线性关系良好(r＞0。99)，平均加样回收率在81。56％～94。08％，RSD在1。57％～3。61％(n=9)，检出限在0。37～0。62 μg·kg-1。结论:该方法简便、准确，可用于中成药及保健品中4种抗痛风类药物成分的测定。
Determination of Four Anti-gout Drugs in Traditional Chinese Medicines and Health-care Products by 2D-LC-MS/MS
Objective:To establish a method for the determination of four anti-gout drugs in traditional Chinese medicines and health-care products by 2D-LC-MS/MS.Methods:The 2D-LC-MS/MS system in-cluded the follows:1D chromatographic column,Agilent Zorbax SB-C18(4.6 mm × 50 mm,5 μm);2D chro-matographic column,Agilent Poroshell 120 EC-C18(2.1 mm × 100 mm,2.7 μm);mobile phase A,0.1％formic acid solution(containing 5 mmol·L-1 ammonium formate);mobile phase B,acetonitrile;gradient elution;col-umn temperature,40℃;injection volume,2 μL;ion source,ESI;positive ion detection mode,and multiple reactions monitoring(MRM)mode.Results:Nabumetone,ketorolac tromethamine,betamethasone and dex-amethasone showed good linear relationships within their own concentration ranges(r＞0.99),and the aver-age recoveries were 81.56％-94.08％,the RSDs were 1.57％-3.61％(n=9),the LODs were 0.37-0.62 μg·kg-1.Conclusion:The method is simple,rapid,accurate and sensitive,which can be used for the determi-nation of four anti-gout drugs in traditional Chinese medicines and health-care products.
2D-LC-MS/MSTraditional Chinese medicinesHealth-care productsAnti-gout drugs
万方数据
维普
