超高效液相色谱-串联质谱法检测食品中酚汀(丁)类物质

Determination of oxyphenisatine and its derivatives in food by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  微量物证食品类鉴定  超高效液相色谱-串联质谱法  非法添加  定量测定

英文关键词:food identification of trace physical evidence  ultra performance liquid chromatography-tandem mass spectrometry  illegally added  quantitative determination

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测食品中新型非法添加物“酚汀(丁)类物质”的分析方法。方法 首先以回收率和精密度为指标，对提取剂的甲醇浓度进行优化，然后在最优的提取条件下以乙腈和含0.1%甲酸的5 mnol/L乙酸铵溶液为流动相进行梯度洗脱，流速为0.3 mL/min，选用ACQUITYUPLC BEH C18色谱柱(100 mm×2.1 mm, 1.7 μm)进行分离，正离子模式下通过多重反应监测模式(multi reaction monitoring, MRM)测定食品中8种酚汀(丁)类物质含量，并验证该方法的线性、延迟效应、基质效应、精密度及准确度。结果 样品经100%甲醇提取后测定得出8种酚汀(丁)类物质在0.5~50.0 ng/mL的线性范围内线性关系良好，相关系数(r)在0.9994~0.9999之间，平均加标回收率在81.35%~96.28%之间，精密度小于10%。本方法中8种酚汀(丁)类物质的检出限为5 μg/kg，定量限为10 μg/kg。结论 本研究建立的检测方法简便准确，可用于食品中非法添加8种酚汀(丁)类物质的定量测定。

英文摘要:

      Objective An analytical method for the detection of "oxyphenisatine and its derivatives", a type of new illegally additives in food, by ultra-high performance liquid chromatography-tandem mass spectrometry was established.. Methods Firstly, the methanol concentration of the extractant was optimized with the recovery rate and precision as indicators. Then, under the optimal extraction conditions, the samples were subjected to gradient elution with acetonitrile and 5 mmol/L ammonium acetate solution containing 0.1% formic acid as mobile phase, gradient elution at a flow rate of 0.3 mL/min. ACQUITYUPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm) was used for separation, and the contents of 8 kinds of oxyphenisatine and its derivatives in food were determined by multiple reaction monitoring(MRM) mode in the positive ion mode(ESI+), and the linearity, delay effect, matrix effect, precision and accuracy of this method were verified.. Results After the samples were extracted with 100% methanol, it was determined that the linear relationship of the 8 kinds of oxyphenisatine and its derivatives was good in the linear range of 0.5 - 50.0 ng/mL, the correlation coefficient (r) was from 0.9994 to 0.9999, the average recovery was from 81.35% to 96.28% , and the precision was less than 10%. The detection limit of 8 kinds of oxyphenisatine and its derivatives in food is 5 μg/kg and the quantitative limit is 10 μg/kg. Conclusion The method is simple and accurate, and can be used for quantitative determination of 8 kinds of oxyphenisatine and its derivatives illegally added in food.