Article(id=1153433738349371918, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153433737141412332, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20241209001, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1733673600000, receivedDateStr=2024-12-09, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1752929632985, onlineDateStr=2025-07-19, pubDate=1745510400000, pubDateStr=2025-04-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1752929632985, onlineIssueDateStr=2025-07-19, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1752929632985, creator=13701087609, updateTime=1752929632985, updator=13701087609, issue=Issue{id=1153433737141412332, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='8', pageStart='1', pageEnd='316', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1752929632696, creator=13701087609, updateTime=1757293087150, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1171735391666225233, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153433737141412332, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1171735391666225234, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153433737141412332, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=282, endPage=287, ext={EN=ArticleExt(id=1153433739657994814, articleId=1153433738349371918, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Rapid determination of chlorate and perchlorate in
Capsicum annuum L. powder by automatic QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry, columnId=1151895321388347923, journalTitle=Journal of Food Safety & Quality, columnName=Food Analysis and Detection, runingTitle=null, highlight=null, articleAbstract=
Objective To establish a detection method for rapid determination of chlorate and perchlorate in Capsicum annuum L. powder by automatic QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods After the sample was centrally weighed, the sample was extracted with a mix-ture of 1% avetic acid-acetonitrile-water (1:1, V:V), and automatic pre-treatment with automatic QuEChERS instrument, the gradient elution was performed by 0.5% formic acid methanol-0.5% formic acid solution, Thermo HYPERCARB as a separation column, gradient elution, series mass spectra electrospray ionization negative mode ionization, multiresponse monitoring pattern detection, qualitative research by the ratio of retention time and ion, the internal standard method was used to qualitative experiment. Results Automatic QuEChERS instrument was used to determine the chlorate and perchlorate of Capsicum annuum L. powder and the pretreatment efficiency was 6 times that of manual. The limits of quantification (S/N=10) were 10 μg/kg, when the spiked level was 10-50 μg/kg (n=6), the sample recoveries for chlorate and perchlorate were 94.0%-96.4%, the relative standard deviations were less than 5%. The calibration curves were linear in the range of 1-100 μg/L with the correlation coefficients above 0.999. Conclusion The method has high automation degree, good accuracy and stability, and the limit of quantitation also meets the requirements of European Union export, can be applied for the determination of chlorate and perchlorate in Capsicum annuum L. powder.
, correspAuthors=Xiao-Wei TIE, 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=Kai ZHOU, Xiao-Wei TIE, Jian FU, Qin-Qin LI, Fa-Ling ZHANG, Xiao-Lin LI), CN=ArticleExt(id=1153433742807917251, articleId=1153433738349371918, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=全自动QuEChERS-超高效液相色谱-串联质谱法快速测定辣椒粉中的氯酸盐及高氯酸盐, 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 建立全自动QuEChERS前处理结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)快速测定辣椒粉中氯酸盐和高氯酸盐的检测方法。方法 样品经集中称量后, 用1%乙酸乙腈-水(1:1, V:V)作为提取溶剂, 利用全自动QuEChERS仪编程后自动前处理, 采用0.5%甲酸甲醇-0.5%甲酸水溶液为流动相, Thermo HYPERCARB为分离柱, 进行梯度洗脱, 串联质谱电喷雾电离源负模式电离, 多反应离子监测模式检测, 以子离子比和保留时间定性, 用内标法定量。结果 采用全自动QuEChERS仪来进行辣椒粉氯酸盐及高氯酸盐的测定前处理效率是人工的6倍, 定量限(S/N=10)为10.0 μg/kg, 加标水平为10~50 μg/kg (n=6)时, 平均回收率为94.0%~96.4%, 相对标准偏差小于5%, 在1~100 μg/L范围内线性关系良好, 相关系数均大于0.999。结论 本方法自动化程度高、准确性及稳定性好, 同时定量限也满足欧盟出口的要求, 适用于出口辣椒粉中氯酸盐及高氯酸盐的测定。
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周凯(1986—), 男, 高级工程师, 主要研究方向为食品安全与检测。E-mail: Kenny.Zhou@ft.eurofinscn.com
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周凯(1986—), 男, 高级工程师, 主要研究方向为食品安全与检测。E-mail: Kenny.Zhou@ft.eurofinscn.com
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DONG YL. Determination of 38 pesticides in nut by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J].
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CHEN XM,
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26(3): 19-24., articleTitle=Determination of chlorate and perchlorate residues in milk and dairy products by ultra performance liquid chromatography-tandem mass spectrometry, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1171733665911455753, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433738349371918, xref=null, ext=[AuthorCompanyExt(id=1171733665915650058, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433738349371918, companyId=1171733665911455753, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Eurofins Technology Service (Qingdao) Co., Ltd., Qingdao 266109, China), AuthorCompanyExt(id=1171733665924038667, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433738349371918, companyId=1171733665911455753, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=欧陆分析检测技术服务(青岛)有限公司, 青岛 266109)])], figs=[ArticleFig(id=1171733669556306011, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433738349371918, language=EN, label=Fig.1, caption=
Total ion chromatogram of chlorate and perchlorate standard solution (10 μg/L), figureFileSmall=7AZL0lraNfhOrNF8E3aOSA==, figureFileBig=Nei4IQkM7BlHxdkc196pig==, tableContent=null), ArticleFig(id=1171733669694718045, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433738349371918, language=CN, label=图1, caption=
氯酸盐和高氯酸盐标准溶液(10 μg/L)的总离子流图, figureFileSmall=7AZL0lraNfhOrNF8E3aOSA==, figureFileBig=Nei4IQkM7BlHxdkc196pig==, tableContent=null), ArticleFig(id=1171733669749243999, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433738349371918, language=EN, label=Table 1, caption=
Program of automatic QuEChERS
, figureFileSmall=null, figureFileBig=null, tableContent=
| 程序 | 动作 | 规格 | 时间/min |
| 步骤1 | 通道1静置前加水溶液 | 10000 μL | 0.1 |
| 步骤2 | 50 mL试管涡旋 | / | 0.6 |
| 步骤3 | 静置 | / | 30.0 |
| 步骤4 | 通道3加溶剂1%乙酸乙腈 | 10000 μL | 0.1 |
| 步骤5 | 50 mL试管振荡 | 500 r/min | 5.0 |
| 步骤6 | 50 mL试管离心 | 4800 r/min | 3.0 |
| 步骤7 | 取上清液 | 3000 μL | 0.1 |
| 步骤8 | 15 mL涡旋 | / | 1.0 |
| 步骤9 | 15 mL试管离心 | 4500 r/min | 1.0 |
), ArticleFig(id=1171733669824741472, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433738349371918, language=CN, label=表1, caption=
全自动QuEChERS仪程序
, figureFileSmall=null, figureFileBig=null, tableContent=
| 程序 | 动作 | 规格 | 时间/min |
| 步骤1 | 通道1静置前加水溶液 | 10000 μL | 0.1 |
| 步骤2 | 50 mL试管涡旋 | / | 0.6 |
| 步骤3 | 静置 | / | 30.0 |
| 步骤4 | 通道3加溶剂1%乙酸乙腈 | 10000 μL | 0.1 |
| 步骤5 | 50 mL试管振荡 | 500 r/min | 5.0 |
| 步骤6 | 50 mL试管离心 | 4800 r/min | 3.0 |
| 步骤7 | 取上清液 | 3000 μL | 0.1 |
| 步骤8 | 15 mL涡旋 | / | 1.0 |
| 步骤9 | 15 mL试管离心 | 4500 r/min | 1.0 |
), ArticleFig(id=1171733669958959202, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433738349371918, language=EN, label=Table 2, caption=
MS conditions for target compound
, figureFileSmall=null, figureFileBig=null, tableContent=
| 中文名称 | CAS | 前体
离子 | 产物
离子 | 去簇
电压/V | 碰撞能
/V | 加速
电压/V |
| 氯酸盐 | 74578-69-1 | 84.8 | 68.8* | 166 | 25 | 4 |
| 82.8 | 66.8 | 166 | 25 | 4 |
| 氯酸盐-内标 | 74578-69-1 | 88.9 | 71* | 166 | 30 | 4 |
| 高氯酸盐 | 74578-69-1 | 98.8 | 82.7* | 166 | 30 | 4 |
| 100.8 | 84.7 | 166 | 30 | 4 |
高氯酸盐-
内标 | 74578-69-1 | 107.0 | 89* | 166 | 30 | 4 |
), ArticleFig(id=1171733670093176931, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433738349371918, language=CN, label=表2, caption=
目标化合物的MS条件
, figureFileSmall=null, figureFileBig=null, tableContent=
| 中文名称 | CAS | 前体
离子 | 产物
离子 | 去簇
电压/V | 碰撞能
/V | 加速
电压/V |
| 氯酸盐 | 74578-69-1 | 84.8 | 68.8* | 166 | 25 | 4 |
| 82.8 | 66.8 | 166 | 25 | 4 |
| 氯酸盐-内标 | 74578-69-1 | 88.9 | 71* | 166 | 30 | 4 |
| 高氯酸盐 | 74578-69-1 | 98.8 | 82.7* | 166 | 30 | 4 |
| 100.8 | 84.7 | 166 | 30 | 4 |
高氯酸盐-
内标 | 74578-69-1 | 107.0 | 89* | 166 | 30 | 4 |
), ArticleFig(id=1171733670399361126, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433738349371918, language=EN, label=Table 3, caption=
Different ratio of extraction solvent for positive sample extraction (n=6)
, figureFileSmall=null, figureFileBig=null, tableContent=
| 提取溶剂 | 高氯酸盐 | 氯酸盐 |
平均值
/(μg/kg) | RSDs
/% | 平均值
/(μg/kg) | RSDs/% |
| 1%乙酸乙腈-水=1:1 (V:V) | 19.9 | 2.54 | 190 | 3.56 |
| 1%乙酸乙腈-水=7:3 (V:V) | 17.5 | 5.06 | 177 | 3.95 |
| 1%乙酸乙腈-水=8:2 (V:V) | 17.1 | 6.47 | 169 | 4.64 |
| 1%乙酸乙腈-水=4:6 (V:V) | 18.4 | 2.90 | 182 | 4.83 |
), ArticleFig(id=1171733670500024425, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433738349371918, language=CN, label=表3, caption=
不同配比提取溶剂针对阳性样品提取情况(n=6)
, figureFileSmall=null, figureFileBig=null, tableContent=
| 提取溶剂 | 高氯酸盐 | 氯酸盐 |
平均值
/(μg/kg) | RSDs
/% | 平均值
/(μg/kg) | RSDs/% |
| 1%乙酸乙腈-水=1:1 (V:V) | 19.9 | 2.54 | 190 | 3.56 |
| 1%乙酸乙腈-水=7:3 (V:V) | 17.5 | 5.06 | 177 | 3.95 |
| 1%乙酸乙腈-水=8:2 (V:V) | 17.1 | 6.47 | 169 | 4.64 |
| 1%乙酸乙腈-水=4:6 (V:V) | 18.4 | 2.90 | 182 | 4.83 |
), ArticleFig(id=1171733670621659243, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433738349371918, language=EN, label=Table 4, caption=
Comparison of manual and automatic QuEChERS (n=6)
, figureFileSmall=null, figureFileBig=null, tableContent=
| 项目 | 人工 | 全自动QuEChERS仪 |
| 每月样品量/个 | 1000 | 1000 |
| 每天样品量/个 | 50 | 50 |
| 检测时长/d | 3.0 | 0.5 |
| 每月人员成本/元 | 6000 | 400 |
| 每月仪器折旧成本/元 | - | 5800 |
| 每月合计成本/元 | 6000 | 6200 |
), ArticleFig(id=1171733670709739628, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433738349371918, language=CN, label=表4, caption=
人工及全自动QuEChERS仪比较(n=6)
, figureFileSmall=null, figureFileBig=null, tableContent=
| 项目 | 人工 | 全自动QuEChERS仪 |
| 每月样品量/个 | 1000 | 1000 |
| 每天样品量/个 | 50 | 50 |
| 检测时长/d | 3.0 | 0.5 |
| 每月人员成本/元 | 6000 | 400 |
| 每月仪器折旧成本/元 | - | 5800 |
| 每月合计成本/元 | 6000 | 6200 |
), ArticleFig(id=1171733670831374446, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433738349371918, language=EN, label=Table 5, caption=
Adding standard recoveries and RSDs of chlorate and perchlorate at different fortification levels (n=6)
, figureFileSmall=null, figureFileBig=null, tableContent=
| 待测物 | 化合物添加水平
/(μg/kg) | 测定平均值
/(μg/kg) | RSDs
/% | 平均
回收率/% |
| 氯酸盐 | 10 | 9.5 | 3.27 | 95.0 |
| 20 | 18.8 | 3.53 | 94.0 |
| 50 | 47.6 | 4.02 | 95.2 |
| 高氯酸盐 | 10 | 9.4 | 3.38 | 94.0 |
| 20 | 19.0 | 3.63 | 95.0 |
| 50 | 48.2 | 4.18 | 96.4 |
), ArticleFig(id=1171733670902677616, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433738349371918, language=CN, label=表5, caption=
不同添加水平下氯酸盐和高氯酸盐的加标回收率和RSDs (n=6)
, figureFileSmall=null, figureFileBig=null, tableContent=
| 待测物 | 化合物添加水平
/(μg/kg) | 测定平均值
/(μg/kg) | RSDs
/% | 平均
回收率/% |
| 氯酸盐 | 10 | 9.5 | 3.27 | 95.0 |
| 20 | 18.8 | 3.53 | 94.0 |
| 50 | 47.6 | 4.02 | 95.2 |
| 高氯酸盐 | 10 | 9.4 | 3.38 | 94.0 |
| 20 | 19.0 | 3.63 | 95.0 |
| 50 | 48.2 | 4.18 | 96.4 |
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