摘要
目的采用超高效液相色谱法-串联质谱法(UHPLC-MS/MS)建立增加骨密度类保健食品中醋氯芬酸的检测方法。方法使用Agilent Eclipse-plus C18色谱柱(2.1 mm×50 mm,1.8μm),流动相为甲醇-10 mmol·L-(16)乙酸铵(含0.1%乙酸)溶液(70∶30)。质谱条件为电喷雾离子源(ESI+),多重反应监测(MRM)方式进行检测。结果醋氯芬酸在5.0~100.0 ng·m L-(16)内与峰面积均呈良好线性关系(r=1.000 0),平均加样回收率为99.1%,RSD为0.25%;重复性RSD为0.4%,最低检测限为1.8μg·kg-(16)。结论该方法灵敏度高,专属性强,定量快速准确,可用于增加骨密度类保健食品中非法添加物醋氯芬酸的检测。
OBJECTIVE To establish a method for detection of aceclofenac in increasing bone density health food by ultra-high performance liquid chromatography-tandem mass spectrometry（UHPLC-MS/MS）. METHODS The separation and analysis was performed on an Agilent Eclipse Plus C18 column（2.1 mm×50 mm, 1.8 μm）. The mobile phase consisted of methanol-0.1% acetic acid containing 10 mmol·L^-1 ammonium acetate（70∶30）. Electrospray ionization（ESI） source was applied and operated in the positive mode. Multiple reaction monitoring（MRM） mode was used to quantify aceclofenac. RESULTS The assay linearity of aceclofenac was confirmed over the range of 5.0^-100.0 ng·m L^-1（r=1.000 0）. The average recovery of aceclofenac was 99.1% and RSD was 0.25%. The repeatability of RSD was 0.4%. The LOQ was 1.8 μg·kg^-1（13） CONCLUSION The method is proved to be specific, sensitive and accurate. Therefore, it can be used to detect aceclofenac illegally added in increasing bone density health food.
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2018年第8期1162-1165,共4页
Chinese Journal of Modern Applied Pharmacy
