摘要
目的：针对抗炎抗风湿功效类中成药，建立可能非法添加的对乙酰氨基酚等10种非甾体抗炎药成分及地塞米松等3种糖皮质激素成分的高效液相色谱-质谱联用的检测方法。方法：色谱柱为PHenomenex LunaC018（2）100A（150mm×2．00mm／／1，3μm）；柱温为40℃；流动相为10mmol／L甲酸铵（以甲酸调节pH值至3．0）及乙腈，梯度洗脱；流速为0．2mL／min；以优化后的质谱参数采集信号。结果：各成分检出限浓度为0．1～2ng／mL；定量限浓度为0．5～5mg／mL；线性范围为各成分定量限～100mg／mL；在线性范围内相关系数均在0．99以上；平均加样回收率为93．0％～102．7％。结论：本方法简便，快速，准确，灵敏度高，专属性好；能用于抗炎抗风湿功效类中成药中非法添加的快速检测。
Objective：To establish a HPLC-MS/MS method for the detection of acetaminophen, dexamethasone and other 10 kinds of non-steroidal anti-inflammatory drugs and 3 kinds of glucocorticoid in anti-inflammatory and antirheumatic traditional Chinese medicines. Methods：PHenomenex Luna C18（2） 100A column （150 mm × 2.00 mm, 3 μm） was used, the column temperature was at 40 ℃, the mobile phase was 10 mmol/L ammonium formate （pH 3.0）-acetonitrile,using gradient elution method, the flow rate was 0.2 mL/min and optimization MS/MS method was adopted. Results：The detection limit of this method was 0.1 ~ 2 ng/mL, the limit of quantitation was 0.5 5 ng/mL and the linear range was the limit of quantitation ~ 100 ng/mL. The test results showed the related coefficient in the linear range was more than 0.99. The average recovery of the method was 93.0% ~ 102.7%. Conclusion：This method is simple, rapid and accurate with a high sensitivity and specificity. It can be used for the quick detection of illegally added materials in anti-inflammatory and antirheumatic traditional Chinese medicines.
出处
《中国执业药师》
CAS
2015年第11期19-26,共8页
China Licensed Pharmacist
关键词
高效液相色谱-质谱联用
抗炎抗风湿功效类中成药
非甾体抗炎药
糖皮质激素
HPLC-MS/MS
Anti-inflammatory and Antirheumatic Traditional Chinese Medicines
Non-steroidal Anti-inflammatory Drug
Glucocorticoid
