微波消解ICP-OES法同时测定香茅草中11种微量元素

doi:10.11924/j.issn.1000-6850.casb19010128

中国农学通报 ›› 2020, Vol. 36 ›› Issue (14): 69-73.doi: 10.11924/j.issn.1000-6850.casb19010128

微波消解ICP-OES法同时测定香茅草中11种微量元素

袁建民¹^,², 何璐¹^,²(), 杨晓琼¹^,², 许智萍¹^,², 孔维喜¹^,²

¹ 云南省农业科学院热区生态农业研究所,云南元谋 651300
² 元谋干热河谷植物园,云南元谋 651300

收稿日期:2019-01-25 修回日期:2019-08-16 出版日期:2020-05-15 发布日期:2020-05-20
通讯作者: 何璐
作者简介:袁建民,男,1984年出生,福建建宁人,助理研究员,硕士,主要从事热带作物资源研究。通信地址：651300 云南省楚雄州元谋县南城街150号云南省农业科学院热区生态农业研究所,Tel：0878-8225661,E-mail： 289980594@qq.com。
基金资助:
国家重点研发计划项目课题“西南干旱河谷特色生物资源利用技术研发”子专题“特色植物资源罗望子与余甘子野生资源开发价值评估及特色品种培育”(2017YFC0505106-1)

Simultaneous Determination of 11 Trace Elements in Cymbopogon citratus by ICP-OES with Microwave Digestion

Yuan Jianmin¹^,², He Lu¹^,²(), Yang Xiaoqiong¹^,², Xu Zhiping¹^,², Kong Weixi¹^,²

¹ Institute of Tropical Eco-agricultural Sciences, Yunnan Academy of Agricultural Sciences, Yuanmou Yunnan 651300
² Dry-hot Valley Botanic Garden, Yuanmou Yunnan 651300

Received:2019-01-25 Revised:2019-08-16 Online:2020-05-15 Published:2020-05-20
Contact: He Lu

摘要/Abstract

摘要：

本研究首次建立了微波消解/电感耦合等离子体发射光谱仪(ICP-OES)同时测定香茅草中11种微量元素(Zn、Cd、Pb、Co、Ni、B、Mn、Fe、Cr、Mg、Cu)的方法,采用HNO₃-H₂O₂混合酸体系进行消解,样品消解完全彻底,并优化了微波消解程序和仪器工作参数。结果表明：待测11种元素的线性关系良好,相关系数(r)为0.9983~0.9999,检出限(LOD)为0.000050~0.081325 mg/L,定量下限(LOQ)为0.0002~0.2455 mg/L。供试样品平均回收率为90.00%~102.50%;相对标准偏差(RSD, n=6)为0.25%~1.64%。元谋和陇川香茅草中不同元素含量之间均存在显著差异,两地香茅草各元素含量高低顺序均为：Mg>Fe>Zn>Mn>Cu>Ni>B,而Cd、Pb、Cr、Co均未检出;同一元素含量在来源地不同的材料间也存在一定差异。该方法具备快速简便、准确度高、灵敏度高、稳定性好等优势,适用于香茅草样品中多元素的同时测定。

关键词: 微波消解, 电感耦合等离子体发射光谱仪(ICP-OES), 香茅草, 检测, 微量元素

Abstract:

In this study, a method was developed for the first time for simultaneous determination of 11 trace elements (Zn, Cd, Pb, Co, Ni, B, Mn, Fe, Cr, Mg, Cu) in Cymbopogon citratus by using inductively coupled plasma optical emission spectrometer (ICP-OES) with microwave digestion. Samples were digested completely by using HNO₃-H₂O₂ mixed acid. The instrumental working parameters and microwave digestion process were optimized. The results showed that: the linear relationship of 11 trace elements was good, the correlative coefficients were in the range of 0.9983-0.9999, the limits of detection (LOD) were in the range of 0.000050-0.081325 mg/L, the limits of quantification (LOQ) were in the range of 0.0002-0.2455 mg/L, the recovery rates were in the range of 90.00%-102.50%, and the relative standard deviations (RSD, n=6) were in the range of 0.25%-1.64%; the concentration of the 11 trace elements in Cymbopogon citratus from Yuanmou and Longchuan had significant differences, the order of was Mg>Fe>Zn>Mn>Cu>Ni>B, and Cd, Pb, Cr and Co were not detected; the concentration of the same element was also different among the samples from different sources. This method has the advantages of rapidness, simplicity, accuracy, high sensitivity and good stability, which is suitable for simultaneous determination of various elements in Cymbopogon citratus.

Key words: microwave digestion, ICP-OES, Cymbopogon citratus, determination, trace elements

中图分类号:

O657.3

袁建民, 何璐, 杨晓琼, 许智萍, 孔维喜. 微波消解ICP-OES法同时测定香茅草中11种微量元素[J]. 中国农学通报, 2020, 36(14): 69-73.

Yuan Jianmin, He Lu, Yang Xiaoqiong, Xu Zhiping, Kong Weixi. Simultaneous Determination of 11 Trace Elements in Cymbopogon citratus by ICP-OES with Microwave Digestion[J]. Chinese Agricultural Science Bulletin, 2020, 36(14): 69-73.

图/表 3

参考文献 26

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元素	检测波长/nm	BEC/(mg/L)	回归方程	相关系数r	检出限LOD/(mg/L)	定量下限LOQ/(mg/L)	RSD/%
Zn	206.200	0.0103009	y=32659.568+754274.11x	0.9997	0.021223	0.0625	1.55
Cd	214.441	0.0067566	y=14483.256+924794.32x	0.9999	0.000050	0.0002	0.31
Pb	220.353	0.1564736	y=1732.4260+2517.224x	0.9999	0.001240	0.0035	0.32
Co	228.615	0.0384767	y=7915.1250+323620.31x	0.9997	0.000152	0.0006	0.20
Ni	231.604	0.0442303	y=20165.023+428508.18x	0.9995	0.003403	0.0100	0.76
B	249.773	0.0567235	y=1349.261+410065.26x	0.9993	0.003325	0.0100	0.84
Mn	257.610	0.0067338	y=131035.44+3870136.0x	0.9999	0.002845	0.0090	0.60
Fe	259.940	0.0243424	y=67485.268+537353.25x	0.9993	0.039154	0.1153	0.85
Cr	267.716	0.3562215	y=97056.226+606.08561x	0.9999	0.024625	0.0735	1.08
Mg	279.553	0.0023844	y=1124979+27451020x	0.9983	0.081325	0.2455	1.05
Cu	324.754	0.0931254	y=31598.023+881367.53x	0.9999	0.010245	0.0332	1.02

元素	检测波长/nm	BEC/(mg/L)	回归方程	相关系数r	检出限LOD/(mg/L)	定量下限LOQ/(mg/L)	RSD/%
Zn	206.200	0.0103009	y=32659.568+754274.11x	0.9997	0.021223	0.0625	1.55
Cd	214.441	0.0067566	y=14483.256+924794.32x	0.9999	0.000050	0.0002	0.31
Pb	220.353	0.1564736	y=1732.4260+2517.224x	0.9999	0.001240	0.0035	0.32
Co	228.615	0.0384767	y=7915.1250+323620.31x	0.9997	0.000152	0.0006	0.20
Ni	231.604	0.0442303	y=20165.023+428508.18x	0.9995	0.003403	0.0100	0.76
B	249.773	0.0567235	y=1349.261+410065.26x	0.9993	0.003325	0.0100	0.84
Mn	257.610	0.0067338	y=131035.44+3870136.0x	0.9999	0.002845	0.0090	0.60
Fe	259.940	0.0243424	y=67485.268+537353.25x	0.9993	0.039154	0.1153	0.85
Cr	267.716	0.3562215	y=97056.226+606.08561x	0.9999	0.024625	0.0735	1.08
Mg	279.553	0.0023844	y=1124979+27451020x	0.9983	0.081325	0.2455	1.05
Cu	324.754	0.0931254	y=31598.023+881367.53x	0.9999	0.010245	0.0332	1.02

元素	元谋香茅草/(mg/kg)	陇川香茅草/(mg/kg)	RSD/%
Zn	65.73c	80.32c	0.50
Cd	ND	ND	0.19
Pb	ND	ND	0.38
Co	ND	ND	0.49
Ni	1.68f	1.25f	3.42
B	0.74g	0.65g	2.85
Mn	28.20d	37.32d	0.98
Fe	158.40b	185.30b	0.72
Cr	ND	ND	0.36
Mg	524.40a	582.36a	0.03
Cu	10.04e	11.35e	1.42

元素	元谋香茅草/(mg/kg)	陇川香茅草/(mg/kg)	RSD/%
Zn	65.73c	80.32c	0.50
Cd	ND	ND	0.19
Pb	ND	ND	0.38
Co	ND	ND	0.49
Ni	1.68f	1.25f	3.42
B	0.74g	0.65g	2.85
Mn	28.20d	37.32d	0.98
Fe	158.40b	185.30b	0.72
Cr	ND	ND	0.36
Mg	524.40a	582.36a	0.03
Cu	10.04e	11.35e	1.42

元素	样品浓度/(mg/L)	样品溶质质量/(μg)	加标值/(μg)	加标后测定值/(mg/L)	加标后溶质质量/(μg)	平均回收率/%	RSD/%
Zn	0.26	1.30	1.0	0.4500	2.2500	95.00	1.64
Cd	0.00	0.00	1.0	0.1870	0.9350	93.50	0.25
Pb	0.00	0.00	1.0	0.1830	0.9150	91.50	1.35
Co	0.00	0.00	1.0	0.1850	0.9250	92.50	0.78
Ni	0.01	0.05	1.0	0.1995	0.9975	94.75	1.26
B	0.00	0.00	1.0	0.1923	0.9615	96.15	1.35
Mn	0.11	0.55	1.0	0.2985	1.4925	94.25	1.21
Fe	0.63	3.15	1.0	0.8288	4.1440	99.40	1.33
Cr	0.00	0.00	1.0	0.1800	0.9000	90.00	1.25
Mg	2.10	10.50	1.0	2.2850	11.4250	92.50	0.76
Cu	0.04	0.20	1.0	0.2450	1.2250	102.50	0.25

微波消解ICP-OES法同时测定香茅草中11种微量元素

Simultaneous Determination of 11 Trace Elements in Cymbopogon citratus by ICP-OES with Microwave Digestion

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