气相色谱法测定黑蒜中两种二烯丙基硫化物含量的不确定度评定  

Evaluation of Uncertainty for Two Diallyl Sulfides in Black Garlic by Gas Chromatography

作　　者：方丽 江晓 杨熙 潘云山 蓝燕玲 FAND Li;JIANG Xiao;YANG Xi;PAN Yunshan;LAN Yanling(Guangdong Provincial Key Laboratory of Chemical Measurement and Emergency Test Technology,Guangdong Provincial Engineering Research Center for Efficacy Component Testing and Risk Substance Rapid Screening of Health Food,Institute of Analysis,Guangdong Academy of Sciences(China National Analytical Center,Guangzhou),Guangdong Guangzhou 510070,China;Guangdong Food and Drug Vocational College,Guangdong Guangzhou 510663,China)

机构地区：[1]广东省科学院测试分析研究所(中国广州分析测试中心),广东省化学测量与应急检测技术重点实验室,广东省保健食品功效成分检测与风险物质快速筛查工程技术研究中心,广东广州510070 [2]广东省食品药品职业技术学校,广东广州510663

出　　处：《饲料工业》2023年第8期106-112,共7页Feed Industry

基　　金：广东省重点领域研发计划项目[2019B020211001]。

摘　　要：试验旨在采用气相色谱法测定黑蒜中两种二烯丙基硫化物的不确定度。黑蒜中的蒜氨酸在一定的p H和温度下转化为二烯丙基三硫醚(DATS)和二烯丙基二硫醚(DADS),经乙醇溶液提取、正己烷萃取后,用带有氢火焰离子化检测器的气相色谱测定,用外标法定量。通过数学建模对两种试验过程中引入的不确定各分量进行分析与评定。结果表明,取消过滤提取液并分取稀释的操作步骤能够有效提高DATS和DADS的测量准确度,并降低结果的分散程度;不确定度主要来源于标准曲线拟合、样品重复性、标准工作溶液配制、样品加标回收率、标准物质纯度。在气相色谱法测定黑蒜中两种二烯丙基硫化物中,应选择合适的标准曲线范围、使用纯度高的标准物质、减少标准溶液的稀释过程、把握过程中的关键控制点,以提高结果的准确性。The aim of this experiment is to evaluate the uncertainty in determination of two diallyl sul⁃fides in black garlin by gas chromatography(GC).Alliin in black garlic is converted into diallyl tri⁃sulfide(DATS)and diallyl disulfide(DADS)at a certain pH and temperature,extracted by ethanol solution and n-hexane successively,determined by GC with hydrogen flame ionization detector,and quantified by external standard method.The uncertainty components introduced by the two experiments were analyzed and evaluated by mathematical modeling.The results showed that the removal of the filtration extract and the separation and dilution pro⁃cedure could improve the measurement accuracy of DATS and DADS effectively and reduce the degree of dispersion of results.The uncertainty is mainly derived from standard curve fitting,sample repeatabili⁃ty,preparation of standard working solution,recovery rate of standard addition and purity of standard sub⁃stance.In the determination of two diallyl sulfides in black garlic by GC,it is necessary to select the ap⁃propriate range of standard curve,use the high purity of the standard material,reduce the dilution pro⁃cess of the standard solution and control the critical control points in the process,so as to improve the accuracy of the results.

关 键 词：黑蒜 二烯丙基三硫醚 二烯丙基二硫醚 不确定度 气相色谱法 

分 类 号：S816.17[农业科学—饲料科学]