超高效液相色谱-三重四级杆串联质谱联用法快速测定冬枣和红枣中的3种甜味剂

Rapid determination of three sweeteners in winter jujube and red dates by ultra-performance liquid chromatography-triple quadrupole tandem mass spectrometry

目的建立一种快速、高效、准确的测定冬枣和红枣中甜蜜素、安赛蜜和糖精钠的超高效液相色谱-三重四级杆串联质谱联用法(UPLC-MS/MS)。方法样品经水稀释后,超声提取,离心后取上清液过膜后上机,采用C18柱分离,MRM负离子模式对3种甜味剂进行检测,基质外标法定量。结果 3种甜味剂在1μg/L~100μg/L内有很好的相关性,相关系数均>0.999,该方法最低检出限为0.002 mg/kg~0.010 mg/kg,最低定量限为0.006 mg/kg~0.030 mg/kg;在0.02 mg/kg和0.2 mg/kg 2种加标水平下,回收率分别在89.4%~98.9%和92.3%~100.6%,相对标准偏差均<10%。结论本方法简便、快速、灵敏,可用于冬枣和红枣中甜蜜素、安赛蜜和糖精钠的同时检测。

Objective To establish a rapid,efficient and accurate method for the determination of cyclamate,acesulfame and saccharin sodium in winter jujube and red dates by ultra-performance liquid chromatography-triple quadrupole tandem mass spectrometry( UPLC-MS/MS). Methods The samples were diluted by water,extracted by ultrasound,centrifuged,and then put on the machine. The three sweeteners were separated by C18 column and tested by MRM negative ion mode. Matrix external standard method was adopted for quantification. Results Three sweeteners have a good correlation within 1 μg/L-100 μg/L,the correlation coefficient is greater than 0. 999,the minimum detection limit is within 0. 002 mg/kg-0. 010 mg/kg,the minimum quantitative limit is within 0. 006 mg/kg-0. 030 mg/kg,the recovery rates are within 89. 4%-98. 9% and92. 3%-100. 6% respectively at the standard addition levels of 0. 02 mg/kg and 0. 2 mg/kg,and the relative standard deviation is less than 10%. Conclusion The method is simple,rapid and sensitive. It can be used for the simultaneous determination of cyclamate,acesulfame and saccharin sodium in winter jujube and red dates.