高清X射线荧光光谱法快速测定干制黑木耳中镉和砷的含量

王一凡; 于铭心; 裴龙英; 赵立艳

doi:10.13386/j.issn1002-0306.2022060260

高清X射线荧光光谱法快速测定干制黑木耳中镉和砷的含量

doi: 10.13386/j.issn1002-0306.2022060260

1.
南京农业大学食品科技学院，江苏南京 210095
2.
新疆理工学院食品科学与工程学院，新疆阿克苏 843100

基金项目: 国家重点研发计划（2019YFC1605400）；六合乡村振兴产业发展项目。

详细信息

作者简介:
王一凡（1997−），女，博士研究生，研究方向：食品营养与安全，E-mail：wangyftt@163.com

通讯作者:
赵立艳（1977−），女，博士，教授，研究方向：食品营养与安全，E-mail：zhlychen@njau.edu.cn

中图分类号: TS207.3
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- 被引次数: 0
出版历程
- 收稿日期: 2022-06-28
- 刊出日期: 2023-05-01

Rapid Detection of Cadmium and Arsenic in Dried Auricularia auricula by High Definition X-ray Fluorescence Spectrometry

1.
College of Food Science and Technology, Nanjing Agricultural University, Nanjing 210095, China
2.
College of Food Science and Engineering, Xinjiang Institute of Technology, Akesu 843100, China

摘要

摘要: 高清X射线荧光（high definition X-ray fluorescence，HDXRF）光谱技术应用于干制黑木耳样品中镉和砷元素的快速检测。将干制黑木耳样品进行前处理，对样品颗粒粒径、样品量和检测时间等因素进行优化，并评价方法的精密度、重复性和稳定性等。结果表明，最优检测条件为：颗粒粒径100目，样品量0.80 g，检测时间600 s。HDXRF法分析样品的总时间不超过15 min。HDXRF法得到的Cd和As的检出限分别为：0.035和0.012 mg/kg。HDXRF法精密度、重复性和稳定性的相对标准偏差（relative standard deviation, RSD）均低于10%。最后对HDXRF法和电感耦合等离子体质谱（inductively coupled plasma mass spectrometry, ICP-MS）法的检测结果进行比较，其结果的相对误差值均小于20%。说明HDXRF法能够满足干制黑木耳中镉和砷快速检测的要求。
- 高清X射线荧光(HDXRF)光谱法 /
- 黑木耳 /
- 镉 /
- 砷 /
- 快速检测
Abstract: The contents of cadmium and arsenic in dried Auricularia auricula were rapidly detected by high definition X-ray fluorescence (HDXRF) spectrometry. In the process of the experiment, the dried Auricularia auricula samples were pre-treated, and the three experimental conditions of particle size, sample weight, and instrument measurement time were optimized. Figures of merit such as precision, reproducibility, and stability were evaluated. The results showed that, the optimal detection conditions of HDXRF were: particle size of 100 meshes, sample weight of 0.80 g, and measurement time of 600 s. This method allowed direct detection of cadmium and arsenic in 15 min, and a detection limit of 0.035 mg/kg of cadmium and 0.012 mg/kg of arsenic, respectively. The relative standard deviations (RSD) of precision, reproducibility and stability of HDXRF were all below 10%. Finally, the results of HDXRF were compared with inductively coupled plasma mass spectrometry (ICP-MS). The results were accurate and the relative errors were less than 20%. It indicates that the method of HDXRF can meet the rapid detection requirements of cadmium and arsenic in dried Auricularia auricula.
- high definition X-ray fluorescence (HDXRF) spectrometry /
- Auricularia auricula /
- cadmium /
- arsenic /
- rapid determination

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图 1 颗粒粒径对HDXRF法检测计数率（a）和元素含量RSD值（b）的影响

注：不同字母表示差异性显著（P<0.05），图2、图3。

Figure 1. Effects of particle size on detection counting rates (a) and RSD values of element content (b) by HDXRF

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图 2 检测时间对HDXRF法检测计数率（a）和元素含量RSD值（b）的影响

Figure 2. Effects of measurement time on detection counting rates (a) and RSD values of element content (b) by HDXRF

下载: 全尺寸图片幻灯片

图 3 样品量对HDXRF法检测计数率（a）和元素含量RSD值（b）的影响

Figure 3. Effects of sample weight on detection counting rates (a) and RSD values of element content (b) by HDXRF

下载: 全尺寸图片幻灯片

表 1 正交试验因素水平表

Table 1. Factors and levels of the orthogonal experiment

水平	因素
水平	A 颗粒粒径（目）	B 样品量（g）	C 检测时间（s）
1	80	0.7	300
2	100	0.8	600
3	120	0.9	900

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表 2 HDXRF法检测计数率的L₉（3⁴）正交试验设计

Table 2. L₉(3⁴) orthogonal test for detection counting rates by HDXRF

试验号		A	B	C	计数率（cps）
试验号		A	B	C	Cd	As
1		1	1	1	602	302
2		1	2	2	1770	789
3		1	3	3	1530	692
4		2	1	2	2075	793
5		2	2	3	2072	642
6		2	3	1	667	421
7		3	1	3	1937	635
8		3	2	1	796	399
9		3	3	2	2028	702
Cd	K₁	3902	4614	2065
	K₂	4814	4638	5873
	K₃	4761	4225	5539
	R	304	138	1269
As	K₁	1783	1730	1122
	K₂	1856	1830	2284
	K₃	1736	1815	1969
	R	40	33	387
优化组合及影响大小		Cd	C₂>A₂>B₂
优化组合及影响大小		As	C₂>A₂>B₂

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表 3 HDXRF法的检出限和定量限测试结果

Table 3. The results of LOD and LOQ of HDXRF

元素	线性范围（mg/kg）	线性方程	相关系数	检出限（mg/kg）	定量限（mg/kg）
Cd	0.12~0.5	Y=1.2030x−0.0182	0.9967	0.035	0.117
As	0.04~0.6	Y=0.8462x+0.0144	0.9971	0.012	0.041

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表 4 HDXRF法的精密度、重复性和稳定性测试结果

Table 4. Precision, repeatability and stability evaluation of HDXRF

元素	Cd	As
精密度（%）	6.34	3.42
重复性（%）	4.29	6.29
稳定性（%）	7.48	5.31

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表 5 ICP-MS法与HDXRF法测试结果比较

Table 5. Comparison of test results between ICP-MS and HDXRF

样品序号	检测方法	元素含量（mg/kg）
样品序号	检测方法	Cd	As
1	ICP-MS	0.217	0.242
	HDXRF	0.19	0.28
	相对误差（%）	−12.4	15.7
2	ICP-MS	0.212	0.069
	HDXRF	0.17	0.08
	相对误差（%）	−18.9	13.0
3	ICP-MS	0.336	0.310
	HDXRF	0.39	0.29
	相对误差（%）	15.2	−6.5
4	ICP-MS	0.184	0.182
	HDXRF	0.21	0.16
	相对误差（%）	12.5	−12.1
5	ICP-MS	0.190	0.587
	HDXRF	0.20	0.51
	相对误差（%）	6.3	−13.5
6	ICP-MS	0.152	0.159
	HDXRF	0.17	0.14
	相对误差（%）	10.5	−10.7

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