摘要
目的:建立准确、灵敏的HPLC-MS/MS方法,检查中药制剂及保健食品中非法添加的6种肾上腺皮质激素类药物。方法:样品经甲醇提取,采用液相色谱/电喷雾离子化质谱法测定。色谱条件:Agilent ZORBAX SB-C18(2.1mm×150mm,3.5μm),柱温35℃,流动相以乙腈-0.1%甲酸溶液进行梯度洗脱,流速:0.25mL/min;质谱条件:以电喷雾电离源正离子模式进行质谱数据采集。结果:6种肾上腺皮质激素药物HPLC图谱分离度良好,质谱分辨率符合鉴别要求。HPLC-MS/MS方法测定上述化学物质的最小检出量为2-14ng。结论:该方法简便,快捷,灵敏度、准确性、重复性均可满足定性检查的要求。
Objective： To develop a high performance liquid hromatography-electrospray ion trap mass spectrometry method for identifying six kinds of corticoid illegally adulterated in traditional Chinese medicine（TCM） preparations and health food ,then provide technical support to enforce the law of administration. Methods： The liquid chromatography-clectrospray ion trap mass spectrometry method was used to detect the samples extracted with methanol. The HPI,C chromatographic determinations were r un on an Waters HPLC/MSD trap using Agilent ZORBAX SB-C18（2.1 mm×150mm,5um）column. The colunm temperature was 30℃. The mobile phase were grading of 0.1% formic acid solution and acetonitrile at a flow rate of 0.25 ml/min.The mass spectrometer conditions were as follows：The fragmentation pattern of these drugs was analyzed by the mass spectrometer after being separated by HPLC, operated in positive ion. Results： A good resolution of six kinds of corticoid were obtained by HPLC and MS. The determination limits were in the range of 2-14 ng. Conclusion：The method is simple, rapid, sensitive and accurate.
出处
《中医药导报》
2009年第5期81-83,共3页
Guiding Journal of Traditional Chinese Medicine and Pharmacy
