高效液相色谱串联质谱法测定白酒中甜蜜素的含量

Determination of sodium cyclamate content in liquor by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  液相色谱-串联质谱法  白酒  甜蜜素

英文关键词:liquid chromatography-tandem mass spectrometry  liquor  sodium cyclamate

中文摘要:

      目的 建立高效液相色谱串联质谱法检测白酒中甜蜜素的分析方法。方法 白酒样品经水浴加热后, 用超纯水定容, 经0.22 μm水相过滤后, 采用10 mmoL/L乙酸铵(A)和甲醇(B)作为流动相进行等度洗脱, 采用高效液相色谱串联三重四极杆质谱仪测定白酒中甜蜜素含量。结果 甜蜜素在0.01~0.50 μg/mL范围内线性关系良好(r2=0.9999), 检出限为0.015 mg/kg, 3个浓度下的加标回收率分别为96.18%、98.44%、92.69%, 相对标准偏差为1.94%~2.11%。结论 该方法灵敏度高、回收率高、检测限低, 适用于白酒中甜蜜素的检测。

英文摘要:

      Objective To establish a method for determination of sodium cyclamate in liquor by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The liquor samples were heated in water bath, fixed volume with ultrapure water, filtered by 0.22 μm water phase, then 10 mmoL/L ammonium acetate (A) and methanol (B) were used as mobile phase for isocratic elution. The content of cyclamate in liquor was detected by high performance liquid chromatography tandem triple quadrupole mass spectrometry. Results Sodium cyclamate had good linear relationships in the range of 0.01-0.50 μg/mL (r2=0.9999), the limit of detection was 0.015 mg/kg. The recoveries at 3 spiked levels were 96.18%, 98.44%, 92.69%, respectively, with the relative standard deviations of 1.94%-2.11%. Conclusion This method has high sensitivity, high recovery, low limit of detection, which is suitable for the determination of sodium cyclamate in liquor.