高效液相色谱法测定饮料中富马酸二甲酯的不确定度评定

Uncertainty evaluation of the determination of dimethyl fumaratein in beverage by high performance liquid chromatography

中文关键词:  不确定度  富马酸二甲酯  高效液相色谱法  饮料

英文关键词:uncertainty  dimethyl fumarate  high performance liquid chromatography  beverage

中文摘要:

      目的 评定高效液相色谱法测定饮料中富马酸二甲酯含量的不确定度。方法 样品经甲醇超声提取, 用水定容, 经色谱柱分离, 流动相等度洗脱, 使用紫外检测器210 nm检测, 外标法定量来测定饮料中富马酸二甲酯的含量。依据JJF 1135-2005《化学分析测量不确定度评定》和JJF 1059.1-2012《测量不确定度评定与表示》, 考察称量、试样定容体积、标准溶液配制、标准曲线拟合、仪器重复测量和回收率等主要因素引入的不确定度, 并对不确定度的各分量进行计算和合成。结果 当饮料中富马酸二甲酯含量为4.64 mg/kg时, 在95%的置信区间下, 其扩展不确定度为0.58 mg/kg(k=2)。评定结果表明, 实验过程中的不确定度主要来源于标准溶液配制、标准曲线拟合。结论 不确定度评定适用于高效液相色谱法快速测定饮料中富马酸二甲酯含量的不确定度分析, 对检测结果准确度的提高具有指导意义。

英文摘要:

      Objective To evaluate the uncertainty in determination of dimethyl fumarate in beverage by high performance liquid chromatography (HPLC). Methods The sample was extracted with methanol, filtered with water, and was analyzed by liquid chromatographic column, with using mobile phase and detected at the wavelength of 210 nm by diode array detector. The target was quantified with external standard curve. According to JJF 1135-2005 Evaluation of uncertainty in chemical analysis measurement and JJF 1059.1-2012 Evaluation and expression of uncertainty in measurement, the factors affecting the determination results were investigated, such as weighing, constant volume, standard curve, measurement repeatability and recovery rate. Meanwhile, each component of uncertainty was calculated and combined. Results When the determination result of dimethyl fumarate in beverage was 4.64 mg/kg, the expand uncertainty was 0.58 mg/kg (k=2) under the confidence interval of 95%. The results showed that the main sources of uncertainty in the determination were standard solution preparation and the standard curve. Conclusion The evaluation of uncertainty method is suitable for analysis of uncertainty of dimethyl fumarate in beverage by HPLC, which is of practical significance for the accuracy of detection result.