硝酸提取-电感耦合等离子质谱法同时测定茶叶中16种元素含量

doi:10.16178/j.issn.0528-9017.20230821

摘要/Abstract

摘要：

建立硝酸提取-微波消解-电感耦合等离子质谱法(ICP-MS)同时测定茶叶中Pb、Cd、As、Cu、Zn、Cr、Co、Mo等16种元素的最佳测定方法。茶叶标准物质GBW10052a(GSB-30a)经微波消解处理后,利用标准曲线法结合在线加入内标溶液,在碰撞模式下分别用外标法和标准加入法同时测定16种元素含量, 研究茶叶基体对待测元素定量分析的影响。结果表明,该方法能同时测定多种元素,线性范围广,所测元素相关系数R² 为0.998~1.000,3个浓度水平添加回收率为88.56%~120.24%,相对标准偏差在0.72%~2.67%,方法检出限0.001~0.200 mg·kg^-1,标准加入法能有效消除基体干扰影响,可用于日常茶叶样品中重金属元素的检测。

关键词: 茶叶, 硝酸, 电感耦合等离子质谱法, 微波, 消解

Abstract:

Establish the optimal determination method for 16 elements including Pb, Cd, As, Cu, Zn, Cr, Co, Mo in tea by nitric acid extraction microwave digestion inductively coupled plasma mass spectrometry (ICP-MS). After microwave digestion of the tea standard substance GBW10052a (GSB-30a), the standard curve method combined with online addition of internal standard solution was used to simultaneously determine the content of 16 elements in collision mode using external standard method and standard addition method. The influence of the tea matrix on the quantitative analysis of the measured elements was studied. The results showed that this method can simultaneously determine multiple elements, with a wide linear range. The correlation coefficient R² of the measured elements is 0.998-1.000. The recovery rates of the three concentration levels added are 88.56%-120.24%, with a relative standard deviation of 0.72%-2.67%. The detection limit of the method is 0.001-0.200 mg·kg^-1. The standard addition method can effectively eliminate the interference of the matrix and can be used for the detection of heavy metal elements in daily tea samples.

Key words: tea, nitric acid, inductively coupled plasma mass spectrometry, microwave, digestion

中图分类号:

S571.1

宁建美, 徐晓安, 唐仕琴, 潘瑛洁. 硝酸提取-电感耦合等离子质谱法同时测定茶叶中16种元素含量[J]. 浙江农业科学, 2024, 65(6): 1457-1462.

NING Jianmei, XU Xiaoan, TANG Shiqin, PAN Yingjie. Simultaneous determination of 16 elements in tea by nitric acid extraction inductively coupled plasma mass spectrometry[J]. Journal of Zhejiang Agricultural Sciences, 2024, 65(6): 1457-1462.

图/表 6

参考文献 9

[1]	胡卫亮. 松阳茶产业全产业链经营的启示与思考[J]. 中国茶叶, 2013, 35(4):14-17.
[2]	鲁照玲, 陈建敏. 有机碳对茶叶中几种重金属定量分析的影响[J]. 环境化学, 2011, 30(11):1963-1964.
[3]	鲁照玲, 姚洪, 陈建敏. ICP-MS对茶叶中6种重金属定量分析方法的研究[J]. 分析仪器, 2012(4):65-70.
[4]	陈红梅, 张滨. ICP-MS法测定茶叶中铅、铬、镉、砷、铜等重金属元素[J]. 食品安全质量检测学报, 2011, 2(4):193-197.
[5]	彭光宇, 王晶, 郑国灿, 等. ICP-MS测定植物中药材中的多种元素[J]. 检验检疫学刊, 2013, 23(3):26-30.
[6]	张中昌, 于青, 王现杰, 等. 微波消解-电感耦合等离子体质谱法测定油井采出液中痕量稀土示踪剂的含量[J]. 理化检验-化学分册, 2022, 58(2):226-228.
[7]	江志鹏, 黄照荣. 电感耦合等离子体质谱法在食品中多元素分析的发展与应用[J]. 食品安全导刊, 2021(18): 180, 182.
[8]	冯睿, 佟岩, 金婉芳, 等. 液相色谱-电感耦合等离子体质谱法测定水产品中的4种形态汞[J]. 食品安全质量检测学报, 2021, 12(1): 137-143.
[9]	叶火香, 刘林敏, 张林福, 等. 松阳茶叶全产业链提升发展建议[J]. 茶业通报, 2014, 36(3):124-126.

步骤	升温时间/ min	功率/ W	恒温温度/ ℃	恒温时间/ min
1	5	800	120	2
2	5	800	150	10
3	5	800	190	15

步骤	升温时间/ min	功率/ W	恒温温度/ ℃	恒温时间/ min
1	5	800	120	2
2	5	800	150	10
3	5	800	190	15

序号	元素	标准系列质量浓度/(μg·L^-1)
序号	元素	STD0	STD1	STD2	STD3	STD4	STD5	STD6	STD7
1	Cd	0.0	0.2	0.5	1.0	2.0	5.0	10.0	20.0
2	As	0.0	0.2	0.5	1.0	2.0	5.0	10.0	20.0
3	Sb	0.0	0.2	0.5	1.0	2.0	5.0	10.0	20.0
4	TI	0.0	0.2	0.5	1.0	2.0	5.0	10.0	20.0
5	V	0.0	0.2	0.5	1.0	2.0	5.0	10.0	20.0
6	Cr	0.0	0.2	0.5	1.0	2.0	5.0	10.0	20.0
7	Co	0.0	0.2	0.5	1.0	2.0	5.0	10.0	20.0
8	Mo	0.0	0.2	0.5	1.0	2.0	5.0	10.0	20.0
9	B	0.0	2.0	5.0	10.0	20.0	50.0	100.0	200.0
10	Ba	0.0	2.0	5.0	10.0	20.0	50.0	100.0	200.0
11	Sr	0.0	2.0	5.0	10.0	20.0	50.0	100.0	200.0
12	Zn	0.0	2.0	5.0	10.0	20.0	50.0	100.0	200.0
13	Pb	0.0	2.0	5.0	10.0	20.0	50.0	100.0	200.0
14	Ni	0.0	2.0	5.0	10.0	20.0	50.0	100.0	200.0
15	Ti	0.0	2.0	5.0	10.0	20.0	50.0	100.0	200.0
16	Cu	0.0	2.0	5.0	10.0	20.0	50.0	100.0	200.0

序号	元素	标准系列质量浓度/(μg·L^-1)
序号	元素	STD0	STD1	STD2	STD3	STD4	STD5	STD6	STD7
1	Cd	0.0	0.2	0.5	1.0	2.0	5.0	10.0	20.0
2	As	0.0	0.2	0.5	1.0	2.0	5.0	10.0	20.0
3	Sb	0.0	0.2	0.5	1.0	2.0	5.0	10.0	20.0
4	TI	0.0	0.2	0.5	1.0	2.0	5.0	10.0	20.0
5	V	0.0	0.2	0.5	1.0	2.0	5.0	10.0	20.0
6	Cr	0.0	0.2	0.5	1.0	2.0	5.0	10.0	20.0
7	Co	0.0	0.2	0.5	1.0	2.0	5.0	10.0	20.0
8	Mo	0.0	0.2	0.5	1.0	2.0	5.0	10.0	20.0
9	B	0.0	2.0	5.0	10.0	20.0	50.0	100.0	200.0
10	Ba	0.0	2.0	5.0	10.0	20.0	50.0	100.0	200.0
11	Sr	0.0	2.0	5.0	10.0	20.0	50.0	100.0	200.0
12	Zn	0.0	2.0	5.0	10.0	20.0	50.0	100.0	200.0
13	Pb	0.0	2.0	5.0	10.0	20.0	50.0	100.0	200.0
14	Ni	0.0	2.0	5.0	10.0	20.0	50.0	100.0	200.0
15	Ti	0.0	2.0	5.0	10.0	20.0	50.0	100.0	200.0
16	Cu	0.0	2.0	5.0	10.0	20.0	50.0	100.0	200.0

序号	元素	线性回归方程	相关系数(R²)	线性范围/(μg·L^-1)	检出限/(mg·kg^-1)
1	¹¹B	Y=2.218x+10.25	0.999	2~200	0.100
2	¹³⁷Ba	Y=98.73x+22.07	1.000	2~200	0.020
3	⁸⁸Sr	Y=88.23x+122.8	1.000	2~200	0.200
4	⁶⁶Zn	Y=23.02x+144.7	0.999	2~200	0.050
5	²⁰⁸Pb	Y=6 702.59x+2 077.52	1.000	2~200	0.020
6	²⁰⁶Pb	Y=1 629.99x+500.34	1.000	2~200	0.020
7	²⁰⁷Pb	Y=1 423.81x+438.57	1.000	2~200	0.020
8	⁶¹Ni	Y=8.611x+3.166	0.999	2~200	0.200
9	⁴⁸Ti	Y=191.55x+123.15	1.000	2~200	0.020
10	⁶³Cu	Y=1 303.58x+920.99	1.000	2~200	0.050
11	¹¹¹Cd	Y=109.4x+8.122	0.998	0.2~20	0.002
12	¹¹⁴Cd	Y=264.3x+2.904	0.999	0.2~20	0.002
13	⁷⁵As	Y=72.77x+2.648	0.999	0.2~20	0.002
14	¹²¹Sb	Y=163.3x+0.676	0.999	0.2~20	0.001
15	²⁰⁵TI	Y=5 154.80x-144.73	1.000	0.2~20	0.001
16	⁵¹V	Y=569.66x+43.25	1.000	0.2~20	0.002
17	⁵²Cr	Y=725.53x+73.34	1.000	0.2~20	0.050
18	⁵³Cr	Y=89.20x+5.27	1.000	0.2~20	0.050
19	⁵⁹Co	Y=1 617.15x+108.45	1.000	0.2~20	0.002
20	⁹⁵Mo	Y=605.01x+6.29	1.000	0.2~20	0.010