Rapid Determination of Multi-Elements in Herb Tea by Semi-Quantitative XRFS and Quantitative ICP-MS
摘 要
采用粉末压片制备花草茶样片,以X射线荧光光谱无标准样品半定量法对5种花草茶样品进行全元素扫描得出所含元素的种类及含量范围;采用微波消解5种花草茶样品,以电感耦合等离子体质谱法进行多种元素的全定量测定。X射线荧光光谱法(XRFS)可以检出5种花草茶样品中质量分数在1 μg·g-1以上的所有金属元素和非金属元素,5种花草茶样品中均测定出钾、磷、硫、镁、钙、氯、硅、铁、锌和锰等10种元素,质量分数最高的元素为钾。根据XRFS测定结果优化电感耦合等离子体质谱法(ICP-MS)仪器工作条件及样品前处理方法。多种元素的质量浓度在一定范围内与其对应的信号强度呈线性关系,方法的检出限(3s)为0.001 8~35.27 μg·kg-1。ICP-MS测定结果与XRFS测定结果一致,砷、铅、镉、铬等4种重金属元素均可被检出。采用XRFS和ICP-MS对柑橘叶国家标准物质(GBW 10020)进行分析,XRFS和ICP-MS的测定值均在认定值范围内,XRFS测定值的相对标准偏差(n=6)均小于5.0%,ICP-MS测定值的相对标准偏差(n=6)均小于3.0%。对XRFS和ICP-MS测定镁、钾、钙、锰、铁、锌等6种金属元素的结果进行对比分析,趋势线斜率为0.761 2~1.306,相关性系数为0.910 8~0.999 8,可比性较好。
Abstract
Semi-quantitative XRFS without standard sample was used to screening all of the elements in samples of five kinds of herb tea to obtain the types and content ranges of the elements contained after using powder pressed method to prepare the sample slice of herb tea. After microwave digestion of herbal tea sample, ICP-MS was applied to quantitative determination of multi-elements. XRFS could detect those metal elements and nonmetal elements which mass fraction more than 1 μg·g-1 in five kinds of herb tea samples. 10 elements, i.e. K, P, S, Mg, Ca, Cl, Si, Fe, Zn and Mn in five kinds of herb tea samples were all detected. The element with the highest mass fraction was K. According to XRFS determination results, the sample pretreatment method and instrument working conditions of ICP-MS were optimized. Linear relationships between values of signal intensity and mass concentration of multi-elements were kept in definite ranges. Detection limits (3s) of the method ranged from 0.001 8 to 35.27 μg·kg-1. Determination results of ICP-MS were consistent with XRFS. 4 heavy metal elements, i.e. As, Pb, Cd and Cr could be detected. The national reference material of citrus leave (GBW 10020) was determined by XRFS and ICP-MS, and determination results of XRFS and ICP-MS were all within the range of the certified values with RSDs (n=6) of determination results of XRFS and ICP-MS were less than 5.0%, 3.0% respectively. Determination results of 6 elements, i.e. Mg, K, Ca, Mn, Fe and Zn by XRFS and ICP-MS were compared. Slopes of trend lines were in the range of 0.761 2-1.306, and correlation coefficients ranged from 0.910 8 to 0.999 8. The two methods were good in comparability.
中图分类号 O657.63 O657.34 DOI 10.11973/lhjy-hx202102007
所属栏目 工作简报
基金项目 华侨大学2019年实验教学与管理改革课题(SY2019Y003)
收稿日期 2019/12/21
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备注吴雅清,博士,主要从事仪器分析与实验室管理工作,wuyaqing@hqu.edu.cn
引用该论文: WU Yaqing. Rapid Determination of Multi-Elements in Herb Tea by Semi-Quantitative XRFS and Quantitative ICP-MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(2): 132~139
吴雅清. X射线荧光光谱法半定量和电感耦合等离子体质谱法全定量快速测定花草茶中多种元素[J]. 理化检验-化学分册, 2021, 57(2): 132~139
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【3】李丹,葛良全,王广西,等.X射线荧光光谱法测定花草茶中22种元素[J].光谱学与光谱分析, 2015,35(7):2043-2048.
【4】HERREROS-CHAVEZ L, CERVERA M L, MORALES-RUBIO A. Direct determination by portable ED-XRF of mineral profile in cocoa powder samples[J]. Food Chemistry, 2019,278:373-379.
【5】黎浩劲,郑咏梅,叶琳,等.电感耦合等离子体质谱法测定饲料中14种主量和痕量元素的含量[J].理化检验-化学分册, 2019,55(1):51-55.
【6】UO M, WADA T, SUGIYAMA T. Applications of X-ray fluorescence analysis (XRF) to dental and medical specimens[J]. Japanese Dental Science Review, 2015,51(1):2-9.
【7】张京京,王莹,赵丹,等.应用ICP-AES同时测定5种花草茶的微量元素[J].沈阳师范大学学报(自然科学版), 2009,27(2):224-226.
【8】孙琳,梁鹏晨,严铸云,等.六种钙类矿物药元素谱的X射线荧光光谱法无标样分析[J].中国实验方剂学杂志, 2018,24(9):70-76.
【9】李霞雪,刘爱平,陈亚,等.微波消解-电感耦合等离子体质谱法测定蔬菜中铬、镉、砷、铅、汞的含量[J].理化检验-化学分册, 2019,55(1):39-45.
【10】刘畅,苑芷茜,薛荔栋,等.ICP-MS与XRF测定PM2.5中重金属含量的对比分析[J].环境科学与技术, 2018,41(4):66-70.
【11】陆金鑫,贾明哲,时超,等.基于无标样定量分析的X射线荧光光谱法快速测定谷物中多种营养元素[J].中国粮油学报, 2016,31(7):138-141.
【12】饶秀勤,应义斌,黄海波,等.基于X射线荧光技术的茶叶产地鉴别方法研究[J].光谱学与光谱分析, 2009,29(3):837-839.
【13】张红梅,王文静.X射线荧光光谱法测定桔梗中的微量元素[J].光谱实验室, 2008(5):925-926.
【14】ONG C C. Direct analysis of plant minerals and comparison of extraction processes using ICP-AES[J]. Food Chemistry, 1992,45:145-149.
【15】古丽克孜·阿日甫,阿力甫·阿不都.ICP-AES法测定新疆玫瑰花中多种元素含量[J].分析测试学报, 2006,25(增刊1):26-28.
【16】王文静,张红梅,李兴元.不同产地金莲花中微量元素的测定[J].广东微量元素科学, 2007(7):36-37.
【17】施敬文,朱晨华,冷桃花,等.电感耦合等离子体质谱法测定花草茶中11种金属元素[J].包装与食品机械, 2013,31(2):67-69.
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