固相萃取-超高效液相色谱-串联质谱法同时检测乳及乳制品中18种甜味剂

Simultaneous determination of 18 kinds of sweeteners in milk and dairy products by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

目的建立固相萃取-超高效液相色谱-串联质谱法测定乳及乳制品中18种甜味剂的检测方法。方法样品采用三乙胺缓冲溶液提取,HLB固相萃取小柱净化,经ACQUITY UPLC®BEH C_(18)色谱柱分离,以5 mmol/L乙酸铵含0.1%(V/V)甲酸水和乙腈溶液为流动相梯度洗脱,外标法定量。结果糖精钠和三氯蔗糖分别在0.050~2.000μg/mL范围内呈现良好的线性关系,其他甜味剂在0.005~0.200μg/mL范围内呈现良好的线性关系,线性相关系数大于0.990,相对标准偏差小于10%,检出限为0.125~1.250 mg/kg,定量限为0.416~4.160 mg/kg,加标回收率为74.8%~114.0%。结论该方法准确、可靠,可快捷准确地对乳及乳制品中的甜味剂的含量进行同时测定。

Objective To establish a method for the determination of 18 kinds of sweeteners in milk and dairy products by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry.Methods The sample was extracted with triethylamine buffer solution,cleaned up by HLB solid phase extraction column,seperated by ACQUITY UPLCBEH C_(18) column using 5 mmol/L ammonium acetate containing 0.1%(V/V)formic acid water and acetonitrile solution as mobile phase,and then quantified by external standard method.Results Saccharin sodium and sucralose showed good linear relationships in the range of 0.050‒2.000μg/mL,respectively,other sweeteners showed good linear relationships in the range of 0.005‒0.200μg/mL,and the linear correlation coefficients were greater than 0.990.The relative standard deviations were less than 10%.The limits of detection were 0.125-1.250 mg/kg,and the limits of quantification were 0.416-4.160 mg/kg,and the recoveries were 74.8%‒114.0%.Conclusion The method is accurate,reliable and can quickly and accurately determine the content of sweetener in milk and dairy products.