测量系统分析在大米镉、铅元素检测中的应用研究

韦冰; 蒋菊媛; 覃均生; 张倩勉

doi:10.16495/j.1006-3757.2023.03.012

测量系统分析在大米镉、铅元素检测中的应用研究

doi: 10.16495/j.1006-3757.2023.03.012

南宁学院食品与质量工程学院，广西南宁　541699

基金项目: 南宁学院专业核心课程建设“测量系统分析”（2021BKHXK08），南宁学院应用型示范课程“质量工程综合实训”（2022XJYYS09）

详细信息

作者简介:
韦冰（1988−），女，硕士，工程师，研究方向为质量统计分析与改进，E-mail：weibingjiayou@163.com

通讯作者:
张倩勉（1981−），女，硕士，高级工程师，研究方向为质量认证及标准化，E-mail：930347555@qq.com

中图分类号: O657. 39
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- 文章访问数: 24
- HTML全文浏览量: 6
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- 被引次数: 0
出版历程
- 收稿日期: 2023-05-15
- 录用日期: 2023-07-20
- 修回日期: 2023-07-20
- 刊出日期: 2023-09-25

Application and Research of Measurement System Analysis for Detection of Cadmium and Lead in Rice

College of Food and Quality Engineering, Nanning University, Nanning 541699, China

Funds: Construction of Core Curriculum of Nanning University "Measurement System Analysis" (2021BKHXK08), Applied Demonstration Course of Nanning University "Quality Engineering Comprehensive Practical Training" (2022XJYYS09)

摘要

摘要: 为提高大米中镉、铅元素检测数据的可靠性，根据GB 5009.12—2017《食品中铅的测定》、GB 5009.15—2014《食品中镉的测定》对大米中镉、铅元素含量进行检测，并以原子吸收分光光度计为测量设备的测量系统进行各类误差分析. 结果表明，两种元素稳定性分析中Xbar控制图均存在超出上下控制界限的点，稳定性不满足要求. 偏倚和线性P值均大于0.05，不存在显著的偏倚和线性误差. 量具研究变异占比（Reproducibility & Repeatability，R&R）分别为54.03%和36.38%，均大于30%，测量误差超出可接受范围. 通过人、机、料、法、环、测等多方面故障排查后稳定性达到统计受控状态，R&R分别降至9.66%和8.95%，均小于10%，测量系统可接受. 利用测量系统分析方法从多方面降低各类测量误差，能够有效保障大米中镉、铅元素含量检测数据的可靠性.
- 测量系统分析 /
- 大米 /
- 镉 /
- 铅 /
- 可靠性
Abstract: In order to improve the reliability of detection data of cadmium and lead elements in rice, the content of cadmium and lead in rice were detected according to GB 5009.12—2017 "Determination of Lead in Food" and GB 5009.15—2014 "Determination of Cadmium in Food", and the various error analysis were carried out for the measuring system analysis (MSA) with the atomic absorption spectrophotometer as measuring equipment. The results showed that the Xbar control charts in the stability analysis of two elements have points beyond the upper and lower control limits, and the stability did not meet the requirements. The bias and linear P values were greater than 0.05, which meant that there were no significant bias and linear error. The results of Reproducibility & Repeatability (R&R) were 54.03% and 36.38%, respectively, both greater than 30%, and the measurement errors were beyond the acceptable range. The stability reached the statistical controlled state after the fault investigation of human, machine, material, method, environment, measurement and other aspects, and the R&R were reduced to 9.66% and 8.95%, respectively, both less than 10%, the measurement system was acceptable. The use of MSA method to reduce various types of measurement errors from many aspects, can effectively guarantee the reliability of the detection data of cadmium and lead contents in rice.
- measurement system analysis /
- rice /
- cadmium /
- lead /
- reliability

HTML全文

图 1 大米镉、铅元素MSA的稳定性分析控制图

（a）（c）镉元素和铅元素的均值图，（b）（d）镉元素和铅元素的极差图

Figure 1. Control charts of stability analysis of MSA for cadmium and lead determinations in rice

(a) (c)Xbar charts of cadmium and lead, respectively, (b) (d) range charts of cadmium and lead, respectively

下载: 全尺寸图片幻灯片

图 2 大米镉、铅元素MSA的稳定性分析控制图（改进后）

（a）（c）镉元素和铅元素的均值图，（b）（d）镉元素和铅元素的极差图

Figure 2. Control charts of stability analysis of MSA for cadmium and lead determinations in rice (after optimization)

(a) (c) Xbar charts of cadmium and lead, respectively, (b) (d) range charts of cadmium and lead, respectively

下载: 全尺寸图片幻灯片

图 3 大米中镉和铅元素MSA的线性和偏倚分析报告

Figure 3. Linear and bias analysis of MSA of cadmium and lead elements in rice

下载: 全尺寸图片幻灯片

图 4 大米中镉、铅元素的部分量具R&R（方差分析）报告

（a）镉元素和（c）铅元素的测量值×样品序号图，（b）镉元素和（d）铅元素的测量值×检测人员图

Figure 4. Part of gage R&R reports (variance analysis) for cadmium and lead detections in rice

(a) (c) measured value × sample number charts of cadmium and lead, respectively, (b) (d) measured value × tester charts of cadmium and lead, respectively

下载: 全尺寸图片幻灯片

表 1 大米镉、铅元素MSA方案设计要点

Table 1. Design points of MSA of cadmium and lead elements in rice

方案要点	研究特性
方案要点	分辨力	稳定性	偏倚和线性	重复性和再现性
样品	—	某一批待测液	覆盖检测范围的5种待测液	覆盖检测范围的5种待测液
子组/个	—	25	5	5
评价人员/人	1	1	1	2
重复测量/次	—	3	12	6
研究方法	十分之一法则	控制图法	独立样件法	方差分析法

下载: 导出CSV

表 2 量具线性分析

Table 2. Linear analysis for gage

自变量	镉			铅
自变量	系数	系数标准误差	P	系数	系数标准误差	P
常量	0.000 123	0.000 301	0.683	0.000 132	0.000 149	0.377
斜率	0.000 323	0.002 674	0.904	−0.000 381	0.002 259	0.867

下载: 导出CSV

表 3 量具偏倚分析

Table 3. Bias analysis for gage

镉			铅
参考值	偏倚	P	参考值	偏倚	P
0.030 0	0.000 150	0.621	0.005 0	0.000 108	0.424
0.090 0 0.105 0 0.120 0 0.170 0	0.000 133 0.000 083 0.000 242 0.000 175	0.607 0.623 0.389 0.565	0.025 0 0.050 0 0.080 0 0.110 0	0.000 083 0.000 192 0.000 133 0.000 042	0.535 0.272 0.551 0.823
平均值	0.000 157	0.183	平均值	0.000 112	0.143

下载: 导出CSV

表 4 改进前后大米中镉、铅元素MSA的变异分析表

Table 4. Analysis results of variation of MSA for cadmium and lead detections in rice before and after improvement

来源	镉		铅
来源	改进前	改进后	改进前	改进后
合计量具R&R/%	54.03	9.66	36.38	8.95
重复性/%	45.67	9.36	28.18	7.09
再现性/%	28.88	2.39	23.01	5.46
样品间误差/%	84.14	99.53	93.15	99.60
合计变异/%	100.00	100.00	100.00	100.00
可区分的类别数	2	14	3	15

下载: 导出CSV

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