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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 |
| 阅读数： | 787 次 |
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