液相色谱-串联质谱法测定白酒中甜蜜素的不确定度评价

Uncertainty evaluation of the determination of sodium cyclamate in liquor by liquid chromatography-tandem mass spectrometry

目的研究液相色谱-串联质谱法测定白酒中甜蜜素的不确定度评定。方法以白酒为例,对GB5009.97-2016中液相色谱-串联质谱法测定甜蜜素的不确定度进行评定。结果白酒中甜蜜素的含量为0.331 mg/kg时,测定结果的合成标准不确定度为0.0242 mg/kg,取k=2,扩展不确定度为0.0484 mg/kg,其结果可表示为(0.331±0.0484)mg/kg。结论测量结果的不确定度主要来源为试样提取液的测定、标准工作液的测定及配制,因此在实际检测工作中,可通过增加平行样和标准工作液的测定次数,提高检测质量。

Objective To investigate the uncertainty evaluation of the determination of sodium cyclamate in liquor by liquid chromatography-tandem mass spectrometry. Methods In the case of liquor, the uncertainty of the determination of sweet element was evaluated by liquid chromatography-tandem mass spectrometry in GB 5009.97-2016. Results When the content of sodium cyclamate in liquor was 0.331 mg/kg, the uncertainty of the determination result was 0.0242 mg/kg, the extended uncertainty was 0.0484 mg/kg with k=2, and the result could be expressed as （0.331＋0.0484） mg/kg. Conclusion The uncertainty of measurement results is mainly derived from the determination of sample extraction solution and the determination and preparation of standard working solution. Therefore, in the actual testing work, the detection quality can be improved by increasing the number of parallel samples and determination time of standard working solution.