顶空-气相色谱法测定橄榄油中六号溶剂残留量的不确定度评定.DOCVIP

顶空-气相色谱法测定橄榄油中六号溶剂残留量的不确定度评定 许蓉蓉* (广西柳州食品药品检验所, 柳州 545004) 摘 要: 目的 评定顶空气相色谱法测定橄榄油中六号溶剂残留量的不确定度。方法运用JJF 1059.1-2012《测量不确定度评定与表示》分析橄榄油中六号溶剂残留量测量过程中的不确定度来源, 通过建立数学模型量化不确定度分量, 计算合成不确定度和扩展不确定度。结果本方法的不确定度主要来源于标准溶液的配制。当橄榄油中六号溶剂残留量为123.6 mg/kg, 扩展不确定度为8.8 mg/kg, 六号溶剂残留量表示为(123.6±8.8) mg/kg(k=2)。结论 该评定方法可为顶空气相色谱法对橄榄油中六号溶剂残留量的测量结果和方法的可靠性提供科学依据。 关键词 Uncertainty evaluation in the determination of No.6 solvent residual in olive oil by headspace gas chromatography XU Rong-Rong* (Liuzhou Institute for Food and Drug Control, Liuzhou 545004, China) ABSTRACT: Objective To evaluate the uncertainty of determination of No.6 solvent residual in olive oil by headspace gas chromatography (HS-GC). Method According to JJF 1059.12-2012 Evaluation and expression of uncertainty in measurement, the uncertainty sources in determination of No.6 solvent residual were analyzed. Furthermore, the combined uncertainty and expanded uncertainty were calculated based on the established mathematic models. Results The major uncertainty source in this method was preparation of standard solution. When the No.6 solvent residual content in olive oil was 123.6 mg/kg, the expanded uncertainty was 8.8 mg/kg, and the No.6 solvent residual content was expressed as (123.6±8.8) mg/kg (k=2). Conclusion The method can provide a scientific basis for the measurement results and the reliability of the method of headspace gas chromatography for the determination of No.6 solvent residual in olive oil. KEY WORDS: headspace gas chromatography; No. 6 solvent; uncertainty; olive oil 1 引 言 橄榄油是世界上唯一以自然状态形式供人类食用的木本植物油, 它完全保存了橄榄油鲜果中的各种营养成分, 被誉为“植物油皇后”、“飘香的软黄金”, 深受人们喜爱[]。国际橄榄油协会将(可食用)橄榄油分为原生橄榄油(virgin olive oil)和精炼橄榄油(lampante olive oil)两大类[]。前者直接从新鲜的橄榄果实中采取机械冷炸的方法榨取, 经过过滤等处理除去异物后得到油汁, 加工过程中完全不经化学处理。后者是通过溶剂浸出法从橄榄油渣中提取并经过精炼而得到[], 市面上销售的普通橄榄油就是精炼油与一定比例的原生橄榄油混合而成, 这类橄榄油有溶剂残留的风险, 我国标准GB 23347-2009[]《橄榄油、油橄榄果渣油》规定, 精炼橄榄油和混合橄榄油均不得检出溶剂残留。为了提供更科学更完整的检测数据, 中国合格评定国家认可委员会要求, 检测实验室应具有并应用评定测量不确定度的程序[]。目前, 已有文献对油茶籽油中六号溶剂的残留量进行不确定度评定[],