超高效液相色谱-串联质谱法检测食品中环己基氨基磺酸钠

Determination of sodium cyclamate in food by ultra performance liquid chromatography-tandem mass spectrometry

目的建立食品中环己基氨基磺酸钠(甜蜜素)的超高效液相色谱一串联质谱(UPL-C-MS/MS)检测方法。方法样品经水溶液溶解,超声提取,高速离心后取上清液供UPLC-MS/MS检测,采用电喷雾电离,负离子扫描,多反应检测模式(MRM),外标法定量。结果环己基氨基磺酸钠的线性范围为1.0~200μg/L,相关系数r≥0.999,最低检出限为0.01 mg/kg。3个不同水平(0.05 mg/kg、0.2 mg/kg和1.0 mg/kg)的加标平均回收率为82.8%~103.5%,相对标准偏差小于10%。结论所建立的方法具有较好的回收率和精密度,准确度和灵敏度高,符合食品中环己基氨基磺酸钠的检测要求,为大通量样品的食品安全检测提供了更灵敏、高效的技术支持。

Objective To establish an ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the determination of sodium cyclamate in food. Methods The samples were extracted with water and ultrasonic-assisted, after high speed centrifuged and determined by UPLC-MS/MS. Identification was achieved by electrospray ionization in negative mode (ESI-) using multiple reaction monitoring (MRM). The quantification was performed by external standard method. Results The sodium cyclamate from 1.0μg/L to 200μg/L showed an excellent linear relationship (r≥0.999). The limit of detection of the sodium cyclamate was 0.01mg/kg. The average recoveries were 82.8%~103.5% at the spiked three concentration levels (add 0.05 mg/kg, 0.2 mg/kg and 1.0 mg/kg). The relative standard deviations (RSD) was less than 10%. Conclusion The established method has a good recovery and precision, high accuracy and sensitivity, and comply with the regulations for the determination of sodium cyclamate in food, provided more sensitive and efficient technical support of the large throughput sample for food safety determination.