UHPLC-MSMS检测增加骨密度保健食品中非法添加物醋氯芬.PDF

UHPLC-MS/MS 检测增加骨密度保健食品中非法添加物醋氯芬酸  陈岑，程巧鸳，周明昊*(浙江省食品药品检验研究院，杭州 310052) 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，1.8 μm) ，流动相为甲醇-10 mmol·L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·mL 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 1.8 μg·kg。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。 关键词：超高效液相色谱- 串联质谱法；醋氯芬酸；增加骨密度；保健食品；非法添加 中图分类号：R917.101 文献标志码：B 文章编号：1007-7693(2018)08-1162-04 DOI: 10.13748/ki.issn1007-7693.2018.08.010 引用本文：陈岑, 程巧鸳, 周明昊. UHPLC-MS/MS 检测增加骨密度保健食品中非法添加物醋氯芬酸[J]. 中国现代应用药 学, 2018, 35(8): 1162-1165. Determination of Aceclofenac Illegally Added in Increasing Bone Density Health Food by UHPLC-MS/MS * CHEN Cen, CHENG Qiaoyuan, ZHOU Minghao (Zhejiang Institute for Food and Drug Control, Hangzhou 310052, China) ABSTRACT: 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 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·mL(r=1.000 0). The average recovery of aceclofenac was 99.1% and RSD was 0