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Article(id=1151437194628575527, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1151437189243089177, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20241211002, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1733846400000, receivedDateStr=2024-12-11, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1752453619867, onlineDateStr=2025-07-14, pubDate=1749916800000, pubDateStr=2025-06-15, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1752453619867, onlineIssueDateStr=2025-07-14, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1752453619867, creator=13701087609, updateTime=1752453619867, updator=13701087609, issue=Issue{id=1151437189243089177, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='11', pageStart='1', pageEnd='320', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1752453618584, creator=13701087609, updateTime=1767768054466, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1215670588966883492, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1151437189243089177, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1215670588966883493, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1151437189243089177, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=245, endPage=250, ext={EN=ArticleExt(id=1151895326949519376, articleId=1151437194628575527, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Determination of total arsenic in food by inductively coupled plasma mass spectrometry, columnId=1151895321388347923, journalTitle=Journal of Food Safety & Quality, columnName=Food Analysis and Detection, runingTitle=null, highlight=null, articleAbstract=

Objective To establish a method for determination of total arsenic in food by inductively coupled plasma mass spectrometry. Methods The 0.3 g of the biological component standard substances, namely rice and spinach, were weighed and digested using a microwave digestion instrument. Then, the collision mode was adopted to reduce the interference of mass spectrometry. The non-mass spectrometry interference was corrected by the internal standard. Acetic acid, isopropanol, methanol and ethanol were selected as sensitizers, and the concentration of the added sensitizers was adjusted and optimized. The response value of arsenic was determined by inductively coupled plasma mass spectrometry. Results The highest arsenic response value was observed at 6% isopropanol content. The established method was applied to analyze certified reference materials and real food samples. The measured values of certified reference materials all fell within their certified values and uncertainty ranges, with relative errors below 2.0%. The limit of detection for total arsenic was 0.0016 mg/kg. Conclusion This method demonstrates straightforward operation, good precision, high accuracy, and a low limit of detection, making it suitable as a reliable analytical approach for determining total arsenic content in various food samples.

, correspAuthors=Ying-Lin GAN, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, authorCompany=null, fund=null, authors=null, authorsList=Chun-Guang MA, Ying-Lin GAN, Zeng-Liang YANG, Zeng-Ming LI, Yu-Huan LI), CN=ArticleExt(id=1151895344309744203, articleId=1151437194628575527, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=电感耦合等离子体质谱法测定食品中总砷, columnId=1151895321958773274, journalTitle=食品安全质量检测学报, columnName=食品分析与检测, runingTitle=null, highlight=null, articleAbstract=

目的 建立电感耦合等离子体质谱法测定食品中总砷。方法 称取0.3 g生物成分标准物质大米和菠菜, 采用微波消解仪进行消解, 然后利用碰撞模式减少质谱干扰, 用内标校正非质谱干扰, 选择乙酸、异丙醇、甲醇、乙醇作为增敏剂, 并调节和优化添加的增敏剂浓度, 用电感耦合等离子体质谱法测定砷的响应值。结果 在异丙醇含量为6%时, 砷元素响应值最高。用建立的方法对食品标准物质及实际样品进行分析, 标准物质测定值均在其认定值及不确定度范围内, 相对误差小于2.0%, 总砷的检出限为0.0016 mg/kg。结论 此方法操作简便、精密度好、准确度高, 检出限低, 可以作为各类食品样品中总砷含量测试方法。

, correspAuthors=甘瑛琳, authorNote=null, correspAuthorsNote=
* 甘瑛琳(1986—), 女, 副主任技师, 主要研究方向为水质、食品和空气环境等样本的理化检验。E-mail:
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马春光(1974—), 男, 副主任技师, 主要研究方向为水质、食品和空气环境等样本的理化检验。E-mail:

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马春光(1974—), 男, 副主任技师, 主要研究方向为水质、食品和空气环境等样本的理化检验。E-mail:

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马春光(1974—), 男, 副主任技师, 主要研究方向为水质、食品和空气环境等样本的理化检验。E-mail:

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tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, language=CN, orderNo=1, keyword=电感耦合等离子体质谱法), Keyword(id=1167030729830572284, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, language=CN, orderNo=2, keyword=増敏剂), Keyword(id=1167030729906069757, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, language=CN, orderNo=3, keyword=总砷)], refs=[Reference(id=1167030731709620493, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, doi=null, pmid=null, pmcid=null, year=2023, volume=13, issue=4, pageStart=311, pageEnd=317, url=null, language=null, rfNumber=[1], rfOrder=0, authorNames=傅志丰, 周鹤, journalName=中国无机分析化学, refType=null, unstructuredReference=傅志丰, 周鹤. 稀酸微波消解-原子荧光光谱法测定大米中总砷[J]. 中国无机分析化学, 2023, 13(4): 311-317., articleTitle=稀酸微波消解-原子荧光光谱法测定大米中总砷, refAbstract=null), Reference(id=1167030731789312270, 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Journal of Food Safety & Quality, 2024, 15(21): 87-92., articleTitle=Comparative study of 2 kinds of pretreatment methods for determination of arsenic, chromium, cadmium and lead in rice flour by inductively coupled plasma mass spectrometry, refAbstract=null)], funds=[Fund(id=1167030731567014156, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, awardId=2021-wjzdx-107, language=CN, fundingSource=青海省卫生健康委指导性课题项目(2021-wjzdx-107), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1167030728345788633, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, xref=null, ext=[AuthorCompanyExt(id=1167030728349982938, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, companyId=1167030728345788633, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Xining Center for Disease Control and Prevention, Xining 810005, China), AuthorCompanyExt(id=1167030728354177243, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, companyId=1167030728345788633, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=西宁市疾病预防控制中心, 西宁 810005)])], figs=[ArticleFig(id=1167030730250002686, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, language=EN, label=Fig.1, caption=Effects of collider gas flow and nebulizer flow on arsenic response (100 μg/L), figureFileSmall=vXBBM5hH6kw1cee5yBSHvg==, figureFileBig=UU2gZCnMH3VZqM/iezNdww==, tableContent=null), ArticleFig(id=1167030730413580543, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, language=CN, label=图1, caption=碰撞气流量和雾化器流量对砷响应值(100 μg/L)的影响, figureFileSmall=vXBBM5hH6kw1cee5yBSHvg==, figureFileBig=UU2gZCnMH3VZqM/iezNdww==, tableContent=null), ArticleFig(id=1167030730484883712, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, language=EN, label=Fig.2, caption=Effects of different sensitizers on arsenic response, figureFileSmall=1uvC0oT1gSX6f03mwrJ6iQ==, figureFileBig=F/Fp3UW6xCPBBpNvwE/rrw==, tableContent=null), ArticleFig(id=1167030730711376129, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, language=CN, label=图2, caption=不同增敏剂对砷响应值的影响, figureFileSmall=1uvC0oT1gSX6f03mwrJ6iQ==, figureFileBig=F/Fp3UW6xCPBBpNvwE/rrw==, tableContent=null), ArticleFig(id=1167030730757513474, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, language=EN, label=Fig.3, caption=Effects of different concentrations of isopropanol on arsenic response, figureFileSmall=52sbFCJW9zHATslFGa/H9A==, figureFileBig=TdJwf3OlUCkX1NeJvN56uA==, tableContent=null), ArticleFig(id=1167030730820428035, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, language=CN, label=图3, caption=不同浓度的异丙醇对砷响应值的影响, figureFileSmall=52sbFCJW9zHATslFGa/H9A==, figureFileBig=TdJwf3OlUCkX1NeJvN56uA==, tableContent=null), ArticleFig(id=1167030730925285636, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, language=EN, label=Table 1, caption=

Working conditions of microwave digester

, figureFileSmall=null, figureFileBig=null, tableContent=
步骤 功率
/W		 爬坡时间/min 控制温度/℃ 保持时间/min
1 1600 5 120 3
2 1600 5 160 5
3 1600 3 185 25
), ArticleFig(id=1167030730979811589, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, language=CN, label=表1, caption=

微波消解仪工作条件

, figureFileSmall=null, figureFileBig=null, tableContent=
步骤 功率
/W		 爬坡时间/min 控制温度/℃ 保持时间/min
1 1600 5 120 3
2 1600 5 160 5
3 1600 3 185 25
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Working parameters for ICP-MS assays

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工作参数 设定值
扫描模式 跳峰
射频功率/W 1100
透镜电压/V 7
辅助气流量/(L/min) 1.20
矩管气体流量/(L/min) 18.00
雾化器流量/(L/min) 0.74
蠕动泵转速/(r/min) 20
), ArticleFig(id=1167030731109835015, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, language=CN, label=表2, caption=

ICP-MS测定的工作参数

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工作参数 设定值
扫描模式 跳峰
射频功率/W 1100
透镜电压/V 7
辅助气流量/(L/min) 1.20
矩管气体流量/(L/min) 18.00
雾化器流量/(L/min) 0.74
蠕动泵转速/(r/min) 20
), ArticleFig(id=1167030731189526792, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, language=EN, label=Table 3, caption=

Experiment on accuracy and precision of total arsenic determination

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质控样品 测定值/(mg/kg) RSDs
/%		 参考值
/(mg/kg)
1 2 3 4 5 6
GSB-1a 0.081 0.082 0.078 0.082 0.079 0.081 2.0 0.08±0.01
GSB-6a 0.582 0.569 0.587 0.584 0.577 0.579 1.1 0.54±0.06
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总砷测定准确度和精密度实验

, figureFileSmall=null, figureFileBig=null, tableContent=
质控样品 测定值/(mg/kg) RSDs
/%		 参考值
/(mg/kg)
1 2 3 4 5 6
GSB-1a 0.081 0.082 0.078 0.082 0.079 0.081 2.0 0.08±0.01
GSB-6a 0.582 0.569 0.587 0.584 0.577 0.579 1.1 0.54±0.06
), ArticleFig(id=1167030731332133130, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437194628575527, language=EN, label=Table 4, caption=

Spiked recovery experiment of total arsenic determination

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元素 本底值
/(mg/kg)		 加标量
/(mg/kg)		 测定总量/(mg/kg) 回收率
/%		 RSDs
/%
砷 0.127 0.05 0.173, 0.176, 0.180, 0.183, 0.179, 0.174 102.0 3.5
0.127 0.10 0.218, 0.233, 0.226, 0.222, 0.229, 0.217 97.0 2.8
0.127 0.20 0.306, 0.309, 0.312, 0.320, 0.324, 0.349 96.5 4.9
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总砷测定加标回收实验

, figureFileSmall=null, figureFileBig=null, tableContent=
元素 本底值
/(mg/kg)		 加标量
/(mg/kg)		 测定总量/(mg/kg) 回收率
/%		 RSDs
/%
砷 0.127 0.05 0.173, 0.176, 0.180, 0.183, 0.179, 0.174 102.0 3.5
0.127 0.10 0.218, 0.233, 0.226, 0.222, 0.229, 0.217 97.0 2.8
0.127 0.20 0.306, 0.309, 0.312, 0.320, 0.324, 0.349 96.5 4.9
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电感耦合等离子体质谱法测定食品中总砷
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马春光 , 甘瑛琳 * , 杨增亮 , 李增明 , 李玉环
食品安全质量检测学报 | 食品分析与检测 2025,16(11): 245-250
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食品安全质量检测学报 | 食品分析与检测 2025, 16(11): 245-250
电感耦合等离子体质谱法测定食品中总砷
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马春光 , 甘瑛琳* , 杨增亮, 李增明, 李玉环
作者信息
  • 西宁市疾病预防控制中心, 西宁 810005

    • 马春光(1974—), 男, 副主任技师, 主要研究方向为水质、食品和空气环境等样本的理化检验。E-mail:

通讯作者:

* 甘瑛琳(1986—), 女, 副主任技师, 主要研究方向为水质、食品和空气环境等样本的理化检验。E-mail:
Determination of total arsenic in food by inductively coupled plasma mass spectrometry
Chun-Guang MA , Ying-Lin GAN* , Zeng-Liang YANG, Zeng-Ming LI, Yu-Huan LI
Affiliations
  • Xining Center for Disease Control and Prevention, Xining 810005, China
出版时间: 2025-06-15 doi: 10.19812/j.cnki.jfsq11-5956/ts.20241211002
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摘要
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目的 建立电感耦合等离子体质谱法测定食品中总砷。方法 称取0.3 g生物成分标准物质大米和菠菜, 采用微波消解仪进行消解, 然后利用碰撞模式减少质谱干扰, 用内标校正非质谱干扰, 选择乙酸、异丙醇、甲醇、乙醇作为增敏剂, 并调节和优化添加的增敏剂浓度, 用电感耦合等离子体质谱法测定砷的响应值。结果 在异丙醇含量为6%时, 砷元素响应值最高。用建立的方法对食品标准物质及实际样品进行分析, 标准物质测定值均在其认定值及不确定度范围内, 相对误差小于2.0%, 总砷的检出限为0.0016 mg/kg。结论 此方法操作简便、精密度好、准确度高, 检出限低, 可以作为各类食品样品中总砷含量测试方法。

电感耦合等离子体质谱法  /  増敏剂  /  总砷

Objective To establish a method for determination of total arsenic in food by inductively coupled plasma mass spectrometry. Methods The 0.3 g of the biological component standard substances, namely rice and spinach, were weighed and digested using a microwave digestion instrument. Then, the collision mode was adopted to reduce the interference of mass spectrometry. The non-mass spectrometry interference was corrected by the internal standard. Acetic acid, isopropanol, methanol and ethanol were selected as sensitizers, and the concentration of the added sensitizers was adjusted and optimized. The response value of arsenic was determined by inductively coupled plasma mass spectrometry. Results The highest arsenic response value was observed at 6% isopropanol content. The established method was applied to analyze certified reference materials and real food samples. The measured values of certified reference materials all fell within their certified values and uncertainty ranges, with relative errors below 2.0%. The limit of detection for total arsenic was 0.0016 mg/kg. Conclusion This method demonstrates straightforward operation, good precision, high accuracy, and a low limit of detection, making it suitable as a reliable analytical approach for determining total arsenic content in various food samples.

inductively coupled plasma mass spectrometry  /  sensitizer  /  total arsenic
马春光, 甘瑛琳, 杨增亮, 李增明, 李玉环. 电感耦合等离子体质谱法测定食品中总砷. 食品安全质量检测学报, 2025 , 16 (11) : 245 -250 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241211002
Chun-Guang MA, Ying-Lin GAN, Zeng-Liang YANG, Zeng-Ming LI, Yu-Huan LI. Determination of total arsenic in food by inductively coupled plasma mass spectrometry[J]. Journal of Food Safety & Quality, 2025 , 16 (11) : 245 -250 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241211002
正文
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0 引言
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随着社会发展和人民生活水平的不断提升, 社会各界对食品安全和健康的重视程度达到新高。而重金属污染问题也逐渐成为公众关注的焦点之一, 长期食用重金属元素污染的食品, 可能引发人体消化系统、肝、肾脏器的损害, 严重的还会影响神经系统和生殖系统, 甚至可能危及生命[1-3]。而砷是一种常见的重金属元素, 现代研究表明过量砷的摄入会引起砷中毒, 长期低量接触也会引起慢性砷中毒, 诱发各种疾病[4]。而土壤污染、添加剂的使用、动植物的富集及食物生产过程中某个环节的不规范等都会造成食物中总砷含量过高[5]。因此, 能够快速准确测定食品中的总砷含量, 对整个食品安全保障和人民群众的身体健康具有非常重要的意义。
目前测定食品中总砷含量的方法主要有电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry, ICP-MS)和原子荧光光谱法。原子荧光光谱法测定样品中总砷, 具有操作简单干扰少和灵敏度高的优势[6], 但对样品的前处理有着较高的要求, 需要加入大量的混合酸进行消解, 消解结束后, 还需进行赶酸处理, 耗时耗力, 且容易引入污染。而ICP-MS在测定过程中无需赶酸, 可以直接测定, 且在稳定性、准确性和灵敏度上更占优势, 成为了当今重金属检测的主流方法[7-8], 已经广泛应用于水、食品及生物材料等的检测分析。而众多研究表明, ICP-MS测定总砷的结果并不一定是完全准确的, 会受到分子离子干扰、同质异位素干扰和基体效应等的干扰, 从而影响测定结果的准确性, 当消解不完全时, 会对砷产生严重的干扰[9-14]。通过查阅文献, 有学者研究ICP-MS在分析含有少量含碳有机试剂时能显著提高高电离能(9~11 eV)元素的电离效率, 且乙醇、异丙醇、乙酸等有机物的加入对砷、硒、碲、汞等元素具有“增敏效应” [15-16]。
目前, 研究并解决ICP-MS测定食品中砷的干扰问题的文献较少。基于此, 本研究采用微波消解法处理食品样品, 利用ICP-MS进行检测, 通过在反应体系中加入增敏剂, 并对增敏剂的种类、浓度及仪器参数进行优化, 为大批量测定食品中总砷提供有利的技术保障。
1 材料与方法
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1.1 材料与试剂
生物成分标准物质(大米)[GBW10010a (GSB-1a)]、生物成分标准物质(菠菜)[GBW10015a (GSB-6a)](中国地质科学院地球物理地球化学勘查研究所)。
硝酸、乙酸、异丙醇、甲醇(优级纯, 德国Merck公司); 乙醇(分析纯, 天津市富宇精细化工有限公司); 砷单元素标准溶液(质量浓度1000 μg/mL, 国家有色金属及电子材料分析测试中心); 内标溶液[质量浓度100 μg/mL, 安捷伦科技(上海)有限公司]; 仪器调谐液铍、铈、铁、铟、锂、镁、铅、铀(质量浓度10 ng/mL, 美国Perkin Elmer公司)。
1.2 仪器与设备
350X型电感耦合等离子体质谱仪、Meinhard型同心雾化器(美国PerkinElmer公司); Milli-IQ7005型超纯水机(德国默克化工技术有限公司); KQ-100DA型数控超声波清洗器(中国昆山市超声仪器有限公司); MARS型微波消解仪(美国CEM公司); LE104E型电子天平(精度0.0001 g, 瑞士梅特勒-托利多仪器有限公司)。
1.3 实验方法
1.3.1 标准储备液的制备
准确吸取砷单元素标准溶液(1000 μg/mL) 1000 μL, 置于100 mL容量瓶中, 用1%硝酸定容, 制得质量浓度为10000 μg/L的砷标准溶液。
1.3.2 标准使用液的制备
准确吸取砷标准储备液(10000 μg/L) 250 μL, 置于25 mL容量瓶中, 用1%硝酸定容, 制得质量浓度为100.00 μg/L的标准使用液。
1.3.3 标准曲线溶液的制备
取0、100、200、800、1000、2000 µL标准使用液, 于10 mL容量瓶中, 用1%硝酸溶液配制成质量浓度为0、1.00、2.00、8.00、10.0、20.00 μg/L的标准系列, 亦可根据样品液中砷元素浓度适当调节标准系列浓度范围。
1.3.4 内标溶液的制备
为了保证实验过程用同一套标准曲线, 本研究选择将增敏剂添加于以在线方式加入的内标溶液中进行测试 (内标与样品进样体积比为1:1)。用百分含量为0%、2%、4%、6%、8%系列的乙酸、异丙醇、甲醇、乙醇, 分别将质量浓度为1000 μg/mL的内标溶液稀释至质量浓度为100 μg/mL。使用前用1%的硝酸稀释成0.050 μg/mL。
1.3.5 样品前处理
准确称取干燥的生物成分标准物质大米和菠菜0.3 g (精确到0.0001 g)于微波消解罐中, 尽量使样品不要黏到罐壁上, 然后加入8 mL硝酸, 拧紧盖子, 静置4 h后, 按照微波消解仪的标准操作步骤进行消解(条件见表1), 消解完成后放至冷却, 然后缓慢开盖排气, 并将消解罐超声脱气, 约10 min后, 将消化后剩余的液转用超纯水少量多次移至50 mL容量瓶中, 混匀备用, 同时做试剂消化空白实验。
1.3.6 电感耦合等离子体质谱仪条件
测定前需使用10 μg/L的调谐液: 铍、铈、铁、铟、锂、镁、铅、铀对仪器进行调谐优化, 使仪器达到最佳状态, 仪器参数见表2。
1.4 数据处理
数据采用Excel 2007软件进行数据统计分析: 测定11份空白样品溶液计算检出限、平行测定6次标准质控样品计算相对标准偏差(relative standard deviation, RSD)等系列数据统计, 采用Origin 2021软件进行响应值与碰撞气流量、响应值与雾化器流量、响应值与浓度等绘制图像。
2 结果与分析
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2.1 仪器条件优化
仪器条件的优化是检测中至关重要的因素, 因此, 在测定前先将仪器调节到砷测定的最佳状态, 保证砷测定的响应值最高, 检出限最低[17-19]。雾化器流量的大小会直接影响雾化产生的气溶胶颗粒的大小和数量, 流量较大时, 通常会产生较小的雾滴粒径, 这有利于样品更好的被质谱仪的进样系统捕获或传输。雾化器流量还会影响气溶胶在质谱仪中的停留时间, 流量较低时, 气溶胶颗粒在仪器中的停留时间较长。所以雾化器流量在一定范围内变大时, 样品提升量会增大, 但增大的幅度显然低于灵敏度的变化, 这是由于雾化器流量增大时, 得到的气溶胶中小粒径的气溶胶比例变多, 而这部分气溶胶是可以使产生信号的有效提升, 从而灵敏度会更显著增大。如图1所示, 随着雾化器流量的增大, 砷的响应值呈现先升高后降低的趋势。当雾化器流量大于0.76 L/min时, 其响应值反而出现下降趋势。
与此同时, 碰撞气流量的过高或过低都会影响到分析物离子和干扰物离子信号, 从而影响砷元素的灵敏度和质谱干扰的去除能力。当雾化器流量一定的情况下, 随着碰撞气流量的增大, 砷的响应值反而降低, 同时, 其检出限也随之降低。
综上所述, 考虑到仪器响应值和检出限, 本方法采用对雾化气及碰撞气流量进行优化, 观察砷质量浓度为100 μg/L溶液的响应值, 得出测试砷元素的最佳雾化器流量为0.76 L/min, 碰撞气流量为0.75 L/min。
2.2 增敏剂种类的选择
大量研究表明, 在ICP-MS测试过程中添加一定比例有机物作为增敏剂能够有效提高第一电离能为9~11 eV元素的响应值[20-23]。本研究在2.1中仪器条件优化的基础上, 探究了不同种类的增敏剂对砷元素响应值强度变化。本研究选择乙酸、异丙醇、乙醇、甲醇等4种有机试剂作为增敏剂, 并添加于在线内标溶液中进行测试, 添加乙酸(4%)、异丙醇(4%)、乙醇(4%)、甲醇(4%)后, 如图2所示, 对砷质量浓度为2、4、8、10、20 μg/L的响应值都有所增加, 说明这几种有机试剂都能达到增敏的效果, 添加4%异丙醇时, 对砷各浓度响应值的增敏效应最强, 分别为无增敏剂存在时的8.3、8.1、7.4、7.1、6.9倍, 且浓度越低, 增敏效应越强, 综上, 本研究优先选择异丙醇作为增敏剂。
2.3 增敏剂浓度的选择
有机物增敏的原理主要有以下几种说法: 有机物的挥发性能有效提高雾化效率; 有机物的存在改变了待测元素在等离子体中离子化的过程, 进而提高了电离效率; 有机物与待测元素离子发生作用, 进而提高了离子的传输效率[24-28]。本研究为进一步优化食品中砷的测定方法, 对异丙醇的浓度进行优化。将异丙醇添加于在线内标溶液中, 使异丙醇浓度为0、2%、4%、6%、8%, 得到砷响应的相应值, 如图3所示。通过此研究发现, 在6%异丙醇存在时, 对砷质量浓度为2、4、8、10、20 μg/L的增敏效应最明显, 是不添加增敏剂时的6.7、6.8、6.1、6.0、6.0倍。当异丙醇浓度高于6%时, 砷的响应值大幅下降, 原因是有机物含量较高, 消耗大量等离子体能量, 从而使离子化效率降低, 导致其响应值下降。综上所述, 本研究中优先选择6%的异丙醇作为增敏剂。
2.4 标准曲线绘制
上述实验表明, 6%的异丙醇对砷的增敏效应效果最佳, 为了进一步验证异丙醇增敏后砷响应值与浓度的线性相关性, 在优化的最佳条件下, 采用标准溶液质量浓度为2、4、8、10、20 μg/L的系列标准使用液。以砷浓度为横坐标, 仪器响应值为纵坐标绘制标准曲线。砷在0~20 μg/L质量浓度范围线性关系良好, 相关系数(r)为0.9996, 线性回归方程为: Y=0.010X+0.002, 满足实验要求。
2.5 检出限实验
制备11份空白样品溶液, 在优化的最佳条件下测定, 得到的3倍标准偏差除以标准曲线斜率, 乘以稀释系数即为方法检出限[1]。计算出方法检出限为0.0016 mg/kg, 定量限为0.0048 mg/kg, 灵敏度比GB 5009.11—2024《食品安全国家标准 食品中总砷及无机砷的测定》高, 可见添加增敏剂, 提高了砷的响应值, 满足方法检出限的要求。
2.6 准确度和精密度实验
为证明该方法的重复性和准确度, 选择两种食品标准样品, 采用本法的微波消解进行前处理后, 定容至50 mL, 在ICP-MS优化的实验条件下, 用6%的异丙醇作为增敏剂的内标溶液, 样品与内标按照体积比1:1进行进样测定, 最终结果的平均值为0.080 mg/kg和0.580 mg/kg, 均在标准样品的参考值范围内, 结果显示该法的准确度能满足实验要求。分别对标准质控样品平行测定6次, 计算RSD, 实验结果显示出良好的精密度, RSDs为1.1%~2.0%(表3)。
2.7 加标回收率实验
为了验证本研究的准确性和实用性, 对某大米样品进行加标回收实验。加标量分别按高、中、低3个浓度水平进行回收实验, 并重复测定6次。结果见表4, 采用添加合适增敏剂后的加标回收率在96.5%~102.0%, RSDs在2.8%~4.9% 符合GB/T 27404—2008《实验室质量控制 规范食品理化检测》的要求, 表明该方法准确度较好, 满足实验要求。
3 讨论与结论
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本研究改进并优化了ICP-MS测定食品中的砷的方法, 该方法线性关系良好, 相关系数均大于0.999, 加标回收率为96.5%~102.0%, RSDs小于5.0%, 检出限为0.0016 mg/kg, 定量限为0.0048 mg/kg, 其线性关系、检出限、定量限、准确度及稳定性等各项指标均能满足实验要求。生物成分标准物质大米和菠菜测定值符合证书标准值不确定范围内, 结果准确稳定。可见本研究有望应用到技术人员的检测实践中, 同时可以为食品风险手册的制定及国家标准的制定提供依据。但此项研究只探讨了有机增敏剂对砷元素的影响, 没有进一步发挥ICP-MS检测多元素的优势[29-30], 下一步将扩大研究范围, 深入研究有机化合物对测定其他元素的影响情况。
基金
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  • 青海省卫生健康委指导性课题项目(2021-wjzdx-107)
文献
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参考文献 引证文献
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20241211002
  • 接收时间：2024-12-11
  • 首发时间：2025-07-14
  • 出版时间：2025-06-15
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  • 收稿日期：2024-12-11
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青海省卫生健康委指导性课题项目(2021-wjzdx-107)
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    西宁市疾病预防控制中心, 西宁 810005

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* 甘瑛琳(1986—), 女, 副主任技师, 主要研究方向为水质、食品和空气环境等样本的理化检验。E-mail:
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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