UPLC-MS/MS法快速筛查抗风湿类中药贴剂中非法添加的17种化学药物成分
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篇名: UPLC-MS/MS法快速筛查抗风湿类中药贴剂中非法添加的17种化学药物成分
TITLE:
摘要: 目的:建立快速筛查抗风湿类中药贴剂中非法添加的9种糖皮质激素和8种非甾体抗炎药物成分的方法。方法:采用超高效液相色谱-串联质谱法(UPLC-MS/MS)。色谱条件:色谱柱Acquity UPLC® BEN C18,流动相为甲醇-水(90 ∶ 10,V/V),流速为0.4 mL/min,柱温为30 ℃,进样量为1 μL;质谱条件:离子源为电喷雾离子源,喷雾针电压为5 500 V,离子源喷雾气GS1、GS2分别为50、50 psi,离子源温度为500 ℃,扫描范围为m/z 50~550,检测方式为正负离子模式,多反应监测(MRM)联合相关信息扫描(IDA)和增强离子扫描(EPI)模式。 结果:17种化学药物成分检测限均≤0.400 μg/mL。精密度、重复性、稳定性试验的RSD分别≤4.93%、7.69%、9.57%。实测样品中可检出双氯芬酸钠。结论:该方法专属性强、灵敏度高,适用于抗风湿类中药贴剂中非法添加化学药物成分的定性分析。
ABSTRACT: OBJECTIVE: To establish a rapid determination method for 9 kinds of glucocorticoid and 8 kinds of non-steroidal anti-inflammatory drugs illegally added into anti-rheumatic TCM patches. METHODS: UPLC-MS/MS method was adopted. The samples were separated on Acquity UPLC® BEN C18 column with methanol-water (90 ∶ 10,V/V) as mobile phase at flow rate 0.4 mL/min. The column temperature was set at 30 ℃, and sample size was 1 μL. The ionization mode was electrospray ion source (ESI): spray needle voltage of 5 500 V, ion source spray GS1, GS2 pressure of 50, 50 psi, ion source temperature of 500 ℃, scanning range of m/z 50-500. The multiple reaction monitoring(MRM)combined with information-dependent acquisition (IDA) and enhanced product ion scanning (EPI) was used to rapid qualitative analysis. RESULTS: The detection limits for 17 kinds of chemical components were not more than 0.400 μg/mL. RSDs for precision, repeatability, stability tests were not more than 4.93%,7.69%,9.57%, respectively. Diclofenac sodium was detected in the sample. CONCLUSIONS: The method is selective and sensitive. It is suitable for qualitative analysis of chemicals illegally added into anti-rheumatism TCM patches.
期刊: 2017年第28卷第12期
作者: 李强,岳磊,李晓静
AUTHORS: LI Qiang,YUE Lei,LI Xiaojing
关键字: 超高效液相色谱-串联质谱法;多反应监测;抗风湿类中药贴剂;非法添加;糖皮质激素;非甾体抗炎药
KEYWORDS: UPLC-MS/MS; MRM; Anti-rheumatism TCM patches; Illegally added; Glucocorticoid; Non-steroidal anti-inflammatory drugs
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