高效液相色谱-质谱法同时测定退热贴中13种解热镇痛类化学药物  

Simultaneous determination of 13 antipyretic and analgesic chemical drugs in antipyretic patches by high-performance liquid chromatography-mass spectrometry

作　　者：傅小红 陈思 姜伟 张思甜 FU Xiaohong;CHEN Si;JIANG Wei;ZHANG Sitian(Nanchang Inspection and Testing Center,Nanchang 330000,China)

机构地区：[1]南昌市检验检测中心,南昌330000

出　　处：《化学分析计量》2024年第6期34-39,共6页Chemical Analysis And Meterage

基　　金：江西省药品监督管理局科研项目(2022JS25)。

摘　　要：建立了高效液相色谱-质谱法同时测定退热贴中13种解热镇痛类化学药物。样品用5 mmol/L甲酸铵溶液(含0.1%的甲酸)-甲醇溶液(体积比为1∶1)提取,经Waters ACQUITY UPLC BEH C_(18)色谱柱(100 mm×2.1 mm,1.7μm)梯度洗脱分离,采用电喷雾离子源,多反应监测模式进行检测,以色谱峰面积外标法进行定量。13种化合物的质量浓度在各自浓度范围内与色谱峰面积呈良好的线性关系,相关系数为0.995~0.9996,方法检出限为0.12~2.5μg/kg,定量限为0.32~8.2μg/kg;基质空白加入不同浓度水平的加标回收率为93.9%~102.0%,测定结果的相对标准偏差为2.31%~4.81%(n=6)。该方法基质干扰小、准确、可靠,适用于退热贴中解热镇痛类化学药非法添加的测定。A method for the simultaneous determination of 13 antipyretic and analgesic chemicals in antipyretic patches by high-performance liquid chromatography-mass spectrometry was established.The samples were extracted with 5 mmol/L ammonium formate containing(0.1%formic acid)with a volume ratio of 1:1 methanol,and separated by gradient elution on a Waters ACQUITY UPLC BEH C_(18) column(100 mm×2.1 mm,1.7μm),then detected with electrospray ion source in multi-reaction monitoring mode,and the chromatographic peak area was used for quantitative analysis with external standard method.There was a good linear relationship between the chromatographic peak area and the concentration of 13 compounds in the each range,with a correlation coefficient of 0.995-0.9996.The detection limits were 0.12-2.5μg/kg;and the quantification limits were 0.32-8.2μg/kg;the recoveries were 93.9%-102.0%and the RSD were 2.31%-4.81%(n=6).The method is accurate,reliable and suitable for the determination of illegal addition of antipyretic and analgesic chemicals in antipyretic patches.

关 键 词：退热贴 解热镇痛 非法添加 高效液相色谱-质谱法 

分 类 号：O657.7[理学—分析化学]