红酒软木塞中愈创木酚残留量的不确定度评定  

Uncertainty Evaluation of Guajacolum in Red Wine Cork Stopper by Headspace Solid-Phasemicroextraction and Gas Chromatographytandem Mass Spectrometry

作　　者：刘继辉 汤丽华 高琳 LIU Jihui;TANG Lihua;GAO Lin(Ningxia Food Testing and Research Institute Key Laboratory of Quality and Safety of Wolf Berry and Wine for State Administration for Market Regulation,Ningxia 750001)

机构地区：[1]宁夏食品检测研究院国家市场监管重点实验室(枸杞和葡萄酒质量安全),宁夏750001

出　　处：《食品工业》2023年第8期323-327,共5页The Food Industry

基　　金：宁夏回族自治区市场监督管理厅科技计划项目(2022SJKY0005)。

摘　　要：分析评定顶空固相微萃取结合气相色谱-串联质谱法测定葡萄酒软木塞中愈创木酚残留量的不确定度。样品经过24 h浸泡提取后,经固相微萃取装置萃取,进入气相色谱进行分离,SIM模式进行检测。依据JJF 10591.1-2012《测量不确定度评定与表示》,过建立合适的数学模拟模型,对主要引入不确定度因素的各分量进行评估和合成。在95%的置信区间下,相对应的软木塞中愈创木酚的含量和扩展不确定度为X=(680±0.158)μg/kg,扩展因子取k=2。此次不确定度评定结果准确可靠,从中分析得出试验过程的不确定度主要来源于标准物质、标准曲线线性拟合、样品测量的重复性,可以通过提高标准物质纯度、优化曲线配制过程和增加加标回收重复性测定次数的方法减少不确定度的引入,从而提高检测数据准确性。Uncertainty evaluation of guajacolum in cork stopper was evaluated by headspace solid-phasemicroextraction and gas chromatography-tandem mass spectrometry.After 24 h of immersion and extraction,the samples were extracted by a solid-phase microextraction device and separated by gas chromatography and detected in SIM mode.The components that mainly introduced uncertainty factors were evaluated and synthesized by establishing a suitable mathematical simulation model according to JJF 10591.1—2012 Evaluation and Presentation of Measurement Uncertainty.At the 95%confidence interval,the content and extension uncertainty of guaiacol in the corresponding cork were X=(680±0.158)μg/kg,and the extension factor was k=2.The uncertainty assessment results were accurate and reliable.The analysis of the uncertainty of the experimental process mainly came from the standard substance,the linear fitting of the standard curve and the repeatability of sample measurement,which could improve the purity of the standard substance,optimize curve preparation process,and increase the spike recovery determination method to reduce the introduction of uncertainty,so as to improve the accuracy of detection data.

关 键 词：不确定度 愈创木酚 软木塞 气相色谱-串联质谱法 

分 类 号：TS262.6[轻工技术与工程—发酵工程] O657.63[轻工技术与工程—食品科学与工程]