超高效液相色谱-串联质谱法检测保健食品中4-甲基咪唑含量
目的 建立超高效液相色谱-串联质谱法测定保健食品中4-甲基咪唑含量的分析方法。方法 样品采用90%乙腈水溶液超声提取后, 提取液经过Waters BEH Hilic色谱柱, 根据亲水作用色谱原理分离待测物, 以0.1%甲酸乙腈-0.1%甲酸水溶液作为流动相洗脱, 正离子电喷雾离子化, 多反应监测模式检测, 超高效液相色谱-串联质谱法(ultra performance liquid chromatography tandem mass spectrometry, UPLC-MS/MS)对样品进行分析。结果 该方法用于4-甲基咪唑检测时, 专属性、精密度和样品稳定性良好, 线性范围在0.11~1.7 ng/mL之间, 相关系数r为0.9998; 加标回收率在94.16%~116.1%之间, 方法准确性良好; 检出限为1 ng/g, 定量限为3 ng/g, 方法灵敏度较好。样品中检出4-甲基咪唑, 含量在12.4~14.9 ng/g之间。结论 该方法专属性强, 准确性好, 灵敏度高, 适用于保健品中4-甲基咪唑的筛查和测定。
Objective To establish a method for determination of 4-methylimidazole in health food by ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted by ultrasonic with 90% acetonitrile water solution. The extracting solution was separated by a Waters BEH Hilic column. According to hydrophilic interaction liquid chromatography theory, the target compound was eluted with 0.1% formic acid acetonitrile and 0.1% formic acid water solution as mobile phase. 4-methylimidazole was ionized by positive electrospray (ESI+), then detected with multiple reaction monitoring mode (MRM), and analyzed by UPLC-MS/MS. Results The specificity, precision and sample stability were satisfactory. The linearity range was 0.11?1.7 ng/mL, and the correlation coefficient was 0.9998. Recoveries were between 94.16% and 116.1%. The limit of detection was 1 ng/g, and limit of quantitation was 3 ng/g. 4-methylimidazole was detected in the testing samples, and the content was in the range of 12.4?14.9 ng/g. Conclusion This method is selective, accurate and sensitive, which is suitable for the screening and determination of 4-methylimidazole in health food
标题：超高效液相色谱-串联质谱法检测保健食品中4-甲基咪唑含量
英文标题：Determination of 4-methylimidazole in health food by ultra performance liquid chromatography tandem mass spectrometry
作者：
钮正睿 中国食品药品检定研究院食品化妆品检定所
赵梅 中国食品药品检定研究院食品化妆品检定所
刘素丽 中国食品药品检定研究院食品化妆品检定所
王宏伟 中国食品药品检定研究院食品化妆品检定所
曹进 中国食品药品检定研究院食品化妆品检定所
中文关键词:超高效液相色谱-串联质谱法,保健食品,4-甲基咪唑,筛查,
英文关键词:ultra performance liquid chromatography tandem mass spectrometry,health food,4- methylimidazole,screening,
发表日期：2019-05-08
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