E-alert
Uncertainty Evaluation for Determination of Aflatoxin M1 in Milk by High Performance Liquid Chromatography Method
-
摘要: 根据方法GB 5009.24-2016《食品安全国家标准食品中黄曲霉毒素M族的测定》，建立高效液相色谱法测定牛奶中黄曲霉毒素M1含量不确定度的数学模型，分析检测过程中的不确定度来源，并对不确定度分量进行量化和合成.当牛奶中黄曲霉毒素M1的质量分数为0.842 μg/kg时，其扩展不确定度为0.048 4 μg/kg（k=2）.方法相对不确定度主要来源于标准品纯度和样品回收率.Abstract: According to the GB 5009.24-2016 method(National food safty standard Determination of Aflatoxin group in food), a mathernatical model of uncertainty evaluation for the determination results of Aflatoxin M1 in milk by high performance liquid chromatography method has been established. The sources of uncertainty for the determination procedure were analyzed and the main uncertainty were quantified and synthesized. When the content of Aflatoxin M1 in milk was 0.842 μg/kg, its extended relative uncertainty was 0.0484 μg/kg(k=2). The major sources of uncertainty were standard purity and recovery rate.
-
Key words:
- Aflatoxin M1 /
- uncertainty /
- high performance liquid chromatography method
-
表 1 标准曲线溶液配制引入的不确定度
Table 1. Uncertainty introduced by standard solution preparation
不确定
度来源项目 A级1 mL
单标线移液管A级1 mL
单标线移液管A级2 mL
单标线移液管A级5 mL
单标线容量瓶A级10 mL
单标线容量瓶刻度误差 允许误差/mL ±0.007 ±0.007 ±0.010 ±0.020 ±0.020 移取体积/mL 1 1 2 5 10 不确定度 0.004 04 0.004 04 0.005 77 0.011 5 0.011 5 温度误差 温度误差/℃ ±3 ±3 ±3 ±3 ±3 膨胀系数/℃-1 1.37×10-3(乙腈) 2.1×10-4(水) 2.1×10-4(水) 2.1×10-4(水) 2.1×10-4(水) 不确定度 0.002 37 0.000 364 0.000 727 0.001 82 0.003 64 相对不确定度 0.004 68 0.004 06 0.002 91 0.002 33 0.001 21 使用次数 1 3 1 2 3 
下载: 导出CSV
表 2 标准曲线溶液拟合引入的不确定度
Table 2. Uncertainty introduced by fitting process of standard curve
质量浓度/(ng/mL) 0.2 0.5 1.0 2.0 5.0 平均质量浓度$ {\bar x}$ (ng/mL) 1.74 峰面积 80.21 176.10 342.52 657.04 1 588.29 标准偏差s 6.66 样品平均质量浓度$ {\bar x}$/(ng/mL) 0.873 不确定度 0.007 86
下载: 导出CSV
表 3 样品回收率
Table 3. Sample recovery
/% 试验次数 1 2 3 4 5 6 回收率 83.82 85.47 91.32 89.65 86.21 87.54 平均回收率R 87.3
下载: 导出CSV
表 4 样品重复测定结果
Table 4. Result of repeated measurement of sample
/(μg/kg) 测定次数 1 2 3 4 5 6 质量分数 0.837 0.840 0.835 0.842 0.849 0.846 平均质量分数X 0.842
下载: 导出CSV
-
[1] 黄亚伟, 魏光, 王若兰, 罗莉.乳品中黄曲霉毒素M1检测方法研究进展[J].食品安全质量检测学报, 2014, 5(3):770-775. http://d.old.wanfangdata.com.cn/Periodical/spaqzljcjs201403024HUANG Ya-wei, WEI Guang, WANG Ruo-lan, Luo Li. Review on detection methods of aflatoxin M1 in dairy products[J]. Journal of food safety and quality, 2014, 5(3):770-775. http://d.old.wanfangdata.com.cn/Periodical/spaqzljcjs201403024 [2] 武瑞霞, 李云姣, 霍超, 王向红, 桑亚新.乳及其乳制品中黄曲霉毒素M1污染及检测技术研究进展[J].中国食品卫生杂志, 2016, 28(1):124-128.WU Ruo-xia, LI Yun-jiao, HUO Chao, WANG Xiang-hong, SANG Ya-xin. Research progress of detection technique and the contamination of aflatoxin M1 in milk and dairy products[J]. Chinese Journal of Food Hygiene, 2016, 28(1):124-128. [3] 梁红, 宋筱瑜, 李凤琴.黄曲霉毒素M1研究进展[J].卫生研究, 2013, 42(6):1055-1058. http://d.old.wanfangdata.com.cn/Periodical/zgggws200604063LIANG Hong, SONG Xiao-yu, LI Feng-qin. Research progress of aflatoxin M1[J]. Journal of Hygiene Research, 2013, 42(6):1055-1058. http://d.old.wanfangdata.com.cn/Periodical/zgggws200604063 [4] GB/T 27025-2008检验和校准实验室能力的通用要求[s].GB/T 27025-2008 General requirements for the competence of testing and calibration laboratories[s]. [5] CNAS-GL006: 2019化学分析中不确定度的评估指南[s].CNAS-GL006-2019 Guidance on quantifying uncertainty in chemical analysis[s]. [6] JJF 1059.1-2012测量不确定度评定与表示[s].JJF 1059.1-2012 Evaluation and expression of uncertainty in measurement[s]. [7] GB 5009.24-2016食品安全国家标准食品中黄曲霉毒素M族的测定[s].GB 5009.24-2016 National food safty standard, Determination of Aflatoxin group in food[s]. [8] JJG196-2006常用玻璃量器检定规程[s].JJG196-2006 Verification regulation of working glass container[s]. -
