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Article(id=1217845647227666457, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217845635080962613, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20250529001, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1748448000000, receivedDateStr=2025-05-29, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1768286628776, onlineDateStr=2026-01-13, pubDate=1756051200000, pubDateStr=2025-08-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1768286628776, onlineIssueDateStr=2026-01-13, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1768286628776, creator=13701087609, updateTime=1768286628776, updator=13701087609, issue=Issue{id=1217845635080962613, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='16', pageStart='1', pageEnd='324', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=1, specialIssue=null, createTime=1768286625881, creator=13701087609, updateTime=1768287480278, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1217849218753024879, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217845635080962613, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1217849218753024880, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217845635080962613, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=94, endPage=99, ext={EN=ArticleExt(id=1217845647680651342, articleId=1217845647227666457, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Contamination and analysis of fusarium and alternaria toxins in wheat and wheat flour in Shaanxi Province, 2022—2024, columnId=1151895322692776479, journalTitle=Journal of Food Safety & Quality, columnName=Special Topic: Analysis and Monitoring of Toxic and Harmful Substances in Food, runingTitle=null, highlight=null, articleAbstract=

Objective To investigate the contamination of fusarium and alternaria toxins in wheat and wheat flour in Shaanxi Province. Methods A total of 140 samples of wheat and wheat flour were randomly collected in circulation of 9 cities from 2022 to 2024. Deoxynivalenol (DON), 3-acetyldeoxynivalenol (3-AcDON), 15-acetyldeoxynivalenol (15-AcDON), nivalenol (NIV), zearalenone (ZEN), tenuazonic acid (TeA), alternariol (AOH), alternariol monomethyl ether (AME) and tentoxin (TEN) were determined by high performance liquid chromatography-tandem mass spectrometry. Results The fusarium and alternaria toxins were detected in wheat and wheat flour. The detection rates of DON, 3-AcDON, 15-AcDON, NIV, ZEN, TeA, TEN, AME in wheat were 83.3% (50/60), 5.00% (3/60), 10.0% (6/60), 11.6% (7/60), 8.33% (5/60), 100% (60/60), 100% (60/60) and 98.3% (59/60), respectively. The detection rates of DON, TeA, TEN, AME in wheat flour were 87.5% (70/80), 96.2% (77/80), 88.7% (71/80) and 63.7% (51/80), respectively. A strong positive correlation between DON and 15-AcDON content was demonstrated in the positive samples, so was between TeA and TEN content. The DON dietary exposure was 959.8 ng/(kg·bw·d), which was less than the corresponding tolerable daily intake value. The TeA, TEN, AME dietary exposures were 159.2, 18.1 and 2.30 ng/(kg·bw·d), which were below the corresponding threshold of toxicological concern values in wheat flour. Conclusion Wheat and wheat flour in Shaanxi Province are generally contaminated with fusarium and alternaria toxins from 2022 to 2024, with the highest detection rates of TeA and TEN, following by DON. The fusarium and alternaria toxins exposure risk of wheat flour are within an acceptable risk range.

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目的 了解陕西省小麦和小麦粉中镰刀菌毒素和交链孢毒素污染情况。方法 2022—2024年在陕西省9个地市随机采集小麦和小麦粉共140份, 采用高效液相色谱-质谱法检测样品中脱氧雪腐镰刀菌烯醇(deoxynivalenol, DON)、3-乙酰脱氧雪腐镰刀菌烯醇(3-acetyldeoxynivalenol, 3-AcDON)、15-乙酰脱氧雪腐镰刀菌烯(15-acetyldeoxynivalenol, 15-AcDON)、雪腐镰刀菌烯醇(nivalenol, NIV)、玉米赤霉烯酮(zearalenone, ZEN)、细交链孢菌酮酸(tenuazonic acid, TeA)、交链孢酚(alternariol, AOH)、交链孢酚单甲醚(alternariol monomethyl ether, AME)、腾毒素(tentoxin, TEN)的含量。结果 陕西省小麦和小麦粉中镰刀菌毒素和交链孢毒素均检出。小麦中DON、3-AcDON、15-AcDON、NIV、ZEN、TeA、TEN和AME的检出率分别为83.3% (50/60)、5.00% (3/60)、10.0% (6/60)、11.6% (7/60)、8.33% (5/60)、100% (60/60)、100% (60/60)和98.3% (59/60)。小麦粉中DON、TeA、TEN和AME的检出率分别为87.5% (70/80)、96.2% (77/80)、88.7% (71/80)和63.7% (51/80)。阳性样品中DON与15-AcDON、TeA与TEN含量之间表现出很强的正相关性。小麦粉DON的膳食暴露量为959.8 ng/(kg·bw·d), 小于每日摄入耐容量值, TeA、TEN、AME的膳食暴露量分别为159.2、18.1和2.30 ng/(kg·bw·d), 小于毒理学关注阈值。结论 2022—2024年陕西省小麦和小麦粉普遍受到镰刀菌毒素和交链孢毒素污染, TeA和TEN检出率最高, DON次之。小麦粉镰刀菌毒素和交链孢毒素的暴露风险处于可接受范围内。

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* 赵迪(1987—), 女, 硕士, 助理研究员, 主要研究方向为食品理化检验。E-mail:
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解宇菲(1993—), 女, 硕士, 研究实习员, 主要研究方向为食品理化检验。E-mail:

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解宇菲(1993—), 女, 硕士, 研究实习员, 主要研究方向为食品理化检验。E-mail:

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Chinese Journal of Public Health, 2018, 34(3): 397-399., articleTitle=Contamination of four Alternaria toxins in wheat flour sampled in Jiangsu Province, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1217864260940644649, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845647227666457, xref=null, ext=[AuthorCompanyExt(id=1217864260953227564, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845647227666457, companyId=1217864260940644649, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Center for Disease Control and Prevention of Shaanxi Province, Xi’an 710054, China), AuthorCompanyExt(id=1217864260970004782, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845647227666457, companyId=1217864260940644649, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=陕西省疾病预防控制中心, 西安 710054)])], figs=[ArticleFig(id=1217864265743123054, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845647227666457, language=EN, label=Table 1, caption=

Distribution of wheat and wheat flour sampling sites

, figureFileSmall=null, figureFileBig=null, tableContent=
地市名称 小麦采样数 小麦粉采样数 小麦粉产地采样数
西安市 9 20 15
铜川市 4 12 10
宝鸡市 9 13 12
咸阳市 11 14 27
渭南市 16 16 13
延安市 0 2 0
汉中市 5 2 0
安康市 2 1 0
商洛市 4 0 0
合计 60 80 80
), ArticleFig(id=1217864265864757879, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845647227666457, language=CN, label=表1, caption=

小麦和小麦粉采样地点分布情况表

, figureFileSmall=null, figureFileBig=null, tableContent=
地市名称 小麦采样数 小麦粉采样数 小麦粉产地采样数
西安市 9 20 15
铜川市 4 12 10
宝鸡市 9 13 12
咸阳市 11 14 27
渭南市 16 16 13
延安市 0 2 0
汉中市 5 2 0
安康市 2 1 0
商洛市 4 0 0
合计 60 80 80
), ArticleFig(id=1217864265973809791, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845647227666457, language=EN, label=Table 2, caption=

Fusarium and alternaria toxins contamination of wheat in Shaanxi Province from 2022 to 2024

, figureFileSmall=null, figureFileBig=null, tableContent=
名称 样品数 平均值/(μg/kg) 浓度范围/(μg/kg) 检出率/%
DON 60 600.00 ND~3210.0 83.3 (50/60)
3-AcDON 60 15.60 ND~35.0 5.00 (3/60)
15-AcDON 60 19.70 ND~81.0 10.0 (6/60)
NIV 60 92.30 ND~456.0 11.6 (7/60)
ZEN 60 8.65 ND~80.8 8.33 (5/60)
TeA 60 128.00 13.3~874.0 100 (60/60)
TEN 60 25.60 2.18~79.5 100 (60/60)
AME 60 29.20 ND~87.5 98.3 (59/60)
), ArticleFig(id=1217864266095444619, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845647227666457, language=CN, label=表2, caption=

2022—2024年陕西省小麦中镰刀菌毒素和交链孢毒素的污染水平

, figureFileSmall=null, figureFileBig=null, tableContent=
名称 样品数 平均值/(μg/kg) 浓度范围/(μg/kg) 检出率/%
DON 60 600.00 ND~3210.0 83.3 (50/60)
3-AcDON 60 15.60 ND~35.0 5.00 (3/60)
15-AcDON 60 19.70 ND~81.0 10.0 (6/60)
NIV 60 92.30 ND~456.0 11.6 (7/60)
ZEN 60 8.65 ND~80.8 8.33 (5/60)
TeA 60 128.00 13.3~874.0 100 (60/60)
TEN 60 25.60 2.18~79.5 100 (60/60)
AME 60 29.20 ND~87.5 98.3 (59/60)
), ArticleFig(id=1217864266221273749, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845647227666457, language=EN, label=Table 3, caption=

Fusarium and alternaria toxins contamination of wheat flour in Shaanxi Province from 2022 to 2024

, figureFileSmall=null, figureFileBig=null, tableContent=
名称 样品数 平均值/(μg/kg) 浓度范围/(μg/kg) 检出率/% 超标率/%
DON 80 267.00 ND~947.00 87.5 (70/80) 0
3-AcDON 80 5.00 ND 0 -
15-AcDON 80 5.00 ND 0 -
NIV 80 17.5 ND 0 -
ZEN 80 2.50 ND 0 0
TeA 80 44.30 ND~167.00 96.2 (77/80) -
TEN 80 5.04 ND~16.00 88.7 (71/80) -
AME 80 0.63 ND~3.29 63.7 (51/80) -
), ArticleFig(id=1217864266355491485, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845647227666457, language=CN, label=表3, caption=

2022—2024年陕西省小麦粉中镰刀菌毒素和交链孢毒素的污染水平

, figureFileSmall=null, figureFileBig=null, tableContent=
名称 样品数 平均值/(μg/kg) 浓度范围/(μg/kg) 检出率/% 超标率/%
DON 80 267.00 ND~947.00 87.5 (70/80) 0
3-AcDON 80 5.00 ND 0 -
15-AcDON 80 5.00 ND 0 -
NIV 80 17.5 ND 0 -
ZEN 80 2.50 ND 0 0
TeA 80 44.30 ND~167.00 96.2 (77/80) -
TEN 80 5.04 ND~16.00 88.7 (71/80) -
AME 80 0.63 ND~3.29 63.7 (51/80) -
), ArticleFig(id=1217864266472932003, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845647227666457, language=EN, label=Table 4, caption=

Correlation analysis of fusarium and alternaria toxins in wheat and wheat flour

, figureFileSmall=null, figureFileBig=null, tableContent=
相关系数 DON 3-AcDON 15-AcDON NIV TeA TEN AME
DON 1 0.554** 0.825** -0.135 -0.014 0.064 0.046
3-AcDON 0.554** 1 0.572** 0.186* 0.061 0.394** -0.243
15-AcDON 0.825** 0.572** 1 -0.121 0.123 0.229** -0.129
NIV -0.135 0.186** -0.121 1 0.237** 0.364** -0.167
TeA -0.014 0.061 0.123 0.237** 1 0.805** -0.127
TEN 0.064 0.394** 0.229** 0.364** 0.805** 1 -0.293**
AME 0.046 -0.243** -0.129 -0.167 -0.127 -0.293** 1
), ArticleFig(id=1217864266581983916, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845647227666457, language=CN, label=表4, caption=

小麦和小麦粉中镰刀菌毒素和交链孢毒素相关性分析

, figureFileSmall=null, figureFileBig=null, tableContent=
相关系数 DON 3-AcDON 15-AcDON NIV TeA TEN AME
DON 1 0.554** 0.825** -0.135 -0.014 0.064 0.046
3-AcDON 0.554** 1 0.572** 0.186* 0.061 0.394** -0.243
15-AcDON 0.825** 0.572** 1 -0.121 0.123 0.229** -0.129
NIV -0.135 0.186** -0.121 1 0.237** 0.364** -0.167
TeA -0.014 0.061 0.123 0.237** 1 0.805** -0.127
TEN 0.064 0.394** 0.229** 0.364** 0.805** 1 -0.293**
AME 0.046 -0.243** -0.129 -0.167 -0.127 -0.293** 1
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2022—2024年陕西省小麦和小麦粉中镰刀菌毒素和交链孢毒素的污染状况及分析
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解宇菲 , 乔海鸥 , 胡佳薇 , 赵迪 *
食品安全质量检测学报 | 专题：食品中有毒有害物质分析与监测 2025,16(16): 94-99
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食品安全质量检测学报 | 专题：食品中有毒有害物质分析与监测 2025, 16(16): 94-99
2022—2024年陕西省小麦和小麦粉中镰刀菌毒素和交链孢毒素的污染状况及分析
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解宇菲 , 乔海鸥, 胡佳薇, 赵迪*
作者信息
  • 陕西省疾病预防控制中心, 西安 710054

    • 解宇菲(1993—), 女, 硕士, 研究实习员, 主要研究方向为食品理化检验。E-mail:

通讯作者:

* 赵迪(1987—), 女, 硕士, 助理研究员, 主要研究方向为食品理化检验。E-mail:
Contamination and analysis of fusarium and alternaria toxins in wheat and wheat flour in Shaanxi Province, 2022—2024
Yu-Fei XIE , Hai-Ou QIAO, Jia-Wei HU, Di ZHAO*
Affiliations
  • Center for Disease Control and Prevention of Shaanxi Province, Xi’an 710054, China
出版时间: 2025-08-25 doi: 10.19812/j.cnki.jfsq11-5956/ts.20250529001
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摘要
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目的 了解陕西省小麦和小麦粉中镰刀菌毒素和交链孢毒素污染情况。方法 2022—2024年在陕西省9个地市随机采集小麦和小麦粉共140份, 采用高效液相色谱-质谱法检测样品中脱氧雪腐镰刀菌烯醇(deoxynivalenol, DON)、3-乙酰脱氧雪腐镰刀菌烯醇(3-acetyldeoxynivalenol, 3-AcDON)、15-乙酰脱氧雪腐镰刀菌烯(15-acetyldeoxynivalenol, 15-AcDON)、雪腐镰刀菌烯醇(nivalenol, NIV)、玉米赤霉烯酮(zearalenone, ZEN)、细交链孢菌酮酸(tenuazonic acid, TeA)、交链孢酚(alternariol, AOH)、交链孢酚单甲醚(alternariol monomethyl ether, AME)、腾毒素(tentoxin, TEN)的含量。结果 陕西省小麦和小麦粉中镰刀菌毒素和交链孢毒素均检出。小麦中DON、3-AcDON、15-AcDON、NIV、ZEN、TeA、TEN和AME的检出率分别为83.3% (50/60)、5.00% (3/60)、10.0% (6/60)、11.6% (7/60)、8.33% (5/60)、100% (60/60)、100% (60/60)和98.3% (59/60)。小麦粉中DON、TeA、TEN和AME的检出率分别为87.5% (70/80)、96.2% (77/80)、88.7% (71/80)和63.7% (51/80)。阳性样品中DON与15-AcDON、TeA与TEN含量之间表现出很强的正相关性。小麦粉DON的膳食暴露量为959.8 ng/(kg·bw·d), 小于每日摄入耐容量值, TeA、TEN、AME的膳食暴露量分别为159.2、18.1和2.30 ng/(kg·bw·d), 小于毒理学关注阈值。结论 2022—2024年陕西省小麦和小麦粉普遍受到镰刀菌毒素和交链孢毒素污染, TeA和TEN检出率最高, DON次之。小麦粉镰刀菌毒素和交链孢毒素的暴露风险处于可接受范围内。

小麦  /  小麦粉  /  镰刀菌毒素  /  交链孢毒素  /  污染

Objective To investigate the contamination of fusarium and alternaria toxins in wheat and wheat flour in Shaanxi Province. Methods A total of 140 samples of wheat and wheat flour were randomly collected in circulation of 9 cities from 2022 to 2024. Deoxynivalenol (DON), 3-acetyldeoxynivalenol (3-AcDON), 15-acetyldeoxynivalenol (15-AcDON), nivalenol (NIV), zearalenone (ZEN), tenuazonic acid (TeA), alternariol (AOH), alternariol monomethyl ether (AME) and tentoxin (TEN) were determined by high performance liquid chromatography-tandem mass spectrometry. Results The fusarium and alternaria toxins were detected in wheat and wheat flour. The detection rates of DON, 3-AcDON, 15-AcDON, NIV, ZEN, TeA, TEN, AME in wheat were 83.3% (50/60), 5.00% (3/60), 10.0% (6/60), 11.6% (7/60), 8.33% (5/60), 100% (60/60), 100% (60/60) and 98.3% (59/60), respectively. The detection rates of DON, TeA, TEN, AME in wheat flour were 87.5% (70/80), 96.2% (77/80), 88.7% (71/80) and 63.7% (51/80), respectively. A strong positive correlation between DON and 15-AcDON content was demonstrated in the positive samples, so was between TeA and TEN content. The DON dietary exposure was 959.8 ng/(kg·bw·d), which was less than the corresponding tolerable daily intake value. The TeA, TEN, AME dietary exposures were 159.2, 18.1 and 2.30 ng/(kg·bw·d), which were below the corresponding threshold of toxicological concern values in wheat flour. Conclusion Wheat and wheat flour in Shaanxi Province are generally contaminated with fusarium and alternaria toxins from 2022 to 2024, with the highest detection rates of TeA and TEN, following by DON. The fusarium and alternaria toxins exposure risk of wheat flour are within an acceptable risk range.

wheat  /  wheat flour  /  fusarium toxins  /  alternaria toxins  /  contamination
解宇菲, 乔海鸥, 胡佳薇, 赵迪. 2022—2024年陕西省小麦和小麦粉中镰刀菌毒素和交链孢毒素的污染状况及分析. 食品安全质量检测学报, 2025 , 16 (16) : 94 -99 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250529001
Yu-Fei XIE, Hai-Ou QIAO, Jia-Wei HU, Di ZHAO. Contamination and analysis of fusarium and alternaria toxins in wheat and wheat flour in Shaanxi Province, 2022—2024[J]. Journal of Food Safety & Quality, 2025 , 16 (16) : 94 -99 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250529001
正文
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0 引言
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镰刀菌毒素是由镰刀菌产生的一类有毒次级代谢产物。小麦赤霉病的主要病原菌就是镰刀菌, 因此小麦很容易受到镰刀菌毒素的污染。交链孢毒素是由丝状真菌交链孢霉产生的一类有毒次级代谢产物。交链孢霉在自然界广泛分布, 是一种腐生菌和植物致病菌, 最常污染小麦、高粱、大麦等谷物。镰刀菌毒素脱氧雪腐镰刀菌烯醇(deoxynivalenol, DON)、3-乙酰脱氧雪腐镰刀菌烯醇(3-acetyldeoxynivalenol, 3-AcDON)、15-乙酰脱氧雪腐镰刀菌烯(15-acetyldeoxynivalenol, 15-AcDON)可引起人体免疫系统失调、消化系统紊乱[1-3], 雪腐镰刀菌烯醇(nivalenol, NIV)具有免疫毒性、基因毒性和生长生殖毒性[4-6], 玉米赤霉烯酮(zearalenone, ZEN)具有很强的生殖毒性和致畸作用[7-8]。交链孢毒素交链孢酚(alternariol, AOH)和交链孢酚单甲醚(alternariol monomethyl ether, AME)具有较强的致突变性和遗传毒性作用[9-11], 细交链孢菌酮酸(tenuazonic acid, TeA)具有细胞毒性和急性毒性[12-13], 腾毒素(tentoxin, TEN)具有植物毒性[14]。陕西是我国农业的发源地之一, 主产粮食作物小麦, 同时陕西饮食以面食为主, 小麦具有十分庞大的消费量, 因此长期监测陕西小麦镰刀菌毒素和交链孢毒素的污染情况十分必要。
根据研究报道[15-19], 小麦易受镰刀菌毒素DON、3-AcDON、15-AcDON、NIV、ZEN和交链孢毒素有TeA、AOH、AME、TEN的侵染。GB 2761—2017《食品安全国家标准 食品中真菌毒素限量》中规定小麦和小麦粉中镰刀菌毒素DON和ZEN的限量值为1000 μg/kg和60 μg/kg。欧盟制定的谷物及其制品中DON的限量标准为750 μg/kg。部分地区开展了谷物中DON和4种交链孢毒素的膳食暴露风险评价, 研究结果显示DON的膳食暴露无显著慢性摄入风险, 但存在急性暴露风险, TeA和TEN、AOH的膳食暴露无显著慢性摄入风险, AME的膳食暴露量水平较高[20-23]。本研究采用高效液相色谱-质谱法测定小麦和小麦粉中镰刀菌毒素和交链孢霉毒素的含量, 分析陕西小麦和小麦粉的污染情况, 为食品安全风险监测和评估提供可靠的数据支持, 为小麦风险预警和防控提供科学依据。
1 材料与方法
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1.1 仪器与试剂
Dionex U3000超高效液相色谱仪(美国赛默飞世尔科技公司); 5500Q-trap三重四极杆串联质谱仪(配电喷雾离子化源和流动注射泵, 美国AB SCIEX公司); Multi ReaX EU涡旋振荡器(美国海道夫公司); SQP分析天平[感量0.1 mg, 赛多利斯科学仪器(北京)有限公司]; MFV-24氮吹仪(广州得泰仪器科技有限公司); CR22N离心机(日本HITACHI公司); Milli-Q型超纯水制备系统(美国Millipore公司); Oasis HLB固相萃取柱(200 mg/6 cc, 美国Waters公司)。
乙腈、甲醇、甲酸(色谱纯, 德国MERCK公司); DON、3-AcDON、15-AcDON、NIV、ZEN(纯度>99%)、TeA、AOH、TEN、AME(质量浓度100 µg/mL)、13C15-DON、13C17-3- AcDON、13C15-NIV、13C18-ZEN、13C14-AOH、13C15-AME、13C10-TeA(质量浓度10.0 µg/mL)、13C17-15-AcDON(质量浓度25.0 µg/mL)(美国Romer公司); TEN-D3(纯度>99%, 加拿大TRC公司)。
1.2 样品采集
2022—2024年在陕西省9个地级市采集小麦60份、小麦粉80份(表1)。小麦采自种植环节。小麦粉采自市售小麦粉供应量大的农贸市场或商超, 样品产地均来自陕西省。每份样品一式两份(1份待检, 1份备样), 实验室粉碎后4 ℃密封保存, 统一检测。
1.3 检测方法
根据《国家食品污染物和有害因素风险监测工作手册》中的食品中真菌毒素多组分测定的标准操作程序[24]。准确称取5.0 g样品(精确至0.001 g)于50 mL离心管, 加入20 mL乙腈-水-甲酸(70:29:1, V:V:V)溶液, 涡旋1 min, 振荡提取30 min, 取1.0 mL提取液至1.5 mL离心管中, 10000 r/min离心5 min。准确移取0.5 mL上清液于另一1.5 mL离心管中, 加入1.0 mL水, 涡旋混匀, 4 ℃下10000 r/min离心5 min, 吸取上清液过0.22 μm滤膜。吸取180 μL样品滤液于300 μL内插管中, 再加入20 μL混合内标溶液(1.25 μg/mL 13C15-DON、13C17-3-AcDON、13C17-15-AcDON、13C15-NIV、13C18-ZEN), 液相色谱-串联质谱法测定镰刀菌毒素的含量。
根据《国家食品污染物和有害因素风险监测工作手册》中的食品中交链孢霉毒素测定的标准操作程序[24]。称取5 g试样(精确至0.001 g)于50 mL刻度离心管中, 加入200 μL混合内标工作液(500 ng/mL TeA-D13、200 ng/mL AOH-D2、20 ng/mL AME-D3、100 ng/mL TEN-D3), 漩涡混匀10 s, 静置过夜。样品加入25 mL磷酸二氢钠-甲醇-乙腈混合提取液, 盖紧盖子, 漩涡混匀10 s, 高速涡旋振荡器上振荡提取15 min, 于4 ℃, 10000 r/min离心10 min, 取5.0 mL上清液, 加入15 mL 0.05 mol/L磷酸二氢钠溶液(pH 3.0), 混匀, 10000 r/min离心10 min, 上清液待净化。HLB固相萃取柱依次用5 mL甲醇和5 mL水活化。将稀释后的样品提取液全部过柱, 再用5 mL 20%甲醇溶液淋洗, 于负压状态下抽干柱子5 min。依次用5 mL甲醇和5 mL乙腈洗脱, 合并洗脱液于小试管中, 45 ℃水浴氮吹近干, 残渣先用200 µL甲醇复溶, 涡旋混匀10 s, 再加1.8 mL水, 涡旋混匀10 s, 于4 ℃, 12000 r/min离心10 min, 液相色谱-串联质谱分析仪上清液测定交链孢霉毒素的含量。
1.4 暴露风险评估
1.4.1 小麦粉的镰刀菌毒素、交链孢霉毒素膳食暴露量
本研究采用点评估方法, 根据公式(1)计算镰刀菌毒素、交链孢霉毒素膳食暴露量。
D=X×C/W
式中: D为镰刀菌毒素、交链孢霉毒素膳食暴露量, ng/(kg·bw·d); X为小麦粉的日均摄入量, g/d; C为小麦粉中镰刀菌毒素、交链孢霉毒素的含量, μg/kg; W为个体体重, 60 kg。
1.4.2 小麦粉膳食中镰刀菌毒素、交链孢霉毒素的暴露风险评估
在镰刀菌毒素膳食暴露量评估基础上, 利用每日摄入耐容量(tolerable daily intake, TDI)来评估镰刀菌毒素长期膳食摄入风险。当D≤TDI时, 表示该污染物的健康风险可以接受, D越小, 风险越小; 当D>TDI时, 表示有不可接受的健康风险, D越大, 风险越大。
在交链孢霉毒素膳食暴露量评估基础上, 利用毒理学关注阈值(threshold of toxicological concern, TTC)评估交链孢毒素的膳食暴露风险。若暴露量D≤TTC值, 说明该污染物的食品安全风险可接受; 若暴露量D>TTC值, 说明该污染物的食品存在一定的安全风险, 需要引起关注。
1.5 数据处理
镰刀菌毒素和交链孢毒素标准曲线的线性方程和结果数据通过AB SCIEX Analyst Software工作站分析得到。采用WPS Office Excel 2023(16120)软件对镰刀菌毒素和交链孢毒素污染水平的实验数据进行处理和分析。参考总膳食研究低水平数据处理办法, 未检出数据的比例小于等于60%, 所有未检出数据用1/2检出限(imit of detection, LOD)替代; 未检出数据的比例高于60%时, 所有未检出数据用LOD替代[21-22,25]。利用SPSS 25.0对小麦和小麦粉中镰刀菌毒素和交链孢毒素含量进行相关性分析及显著性分析。
2 结果与分析
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2.1 线性范围、检出限及加标回收率
DON在1.00~200 ng/mL质量浓度范围的线性方程为Y=0.0539X+0.00643, r=0.9978; 3-AcDON在1.00~200 ng/mL质量浓度范围的线性方程为Y=0.0632X-0.0203, r=0.9978; 15-AcDON在1.00~200 ng/mL质量浓度范围的线性方程为Y=0.0237X-0.0282, r=0.9988; NIV在5.00~200 ng/mL质量浓度范围的线性方程为Y=0.0211X-0.0144, r=0.9983; ZEN在0.50~50.0 ng/mL质量浓度范围的线性方程为Y=7.32e+004X-2.25e+003, r=0.9963。DON、3-AcDON、15-AcDON、NIV和ZEN的检出限为10.0、10.0、10.0、35.0和5.00 μg/kg。分析过程通过加标回收实验和平行双样控制分析质量, 每10个样做一个平行样, 每批样品做一个空白样和样品加标。加标回收实验的回收率为91.2%~109.5%, 平行双样的相对标准偏差(relative standard deviation, RSD)小于10%。
TeA在4.00~200 ng/mL质量浓度范围的线性方程为Y=0.0751X-0.0325, r=0.9996; TEN在0.20~10.0 ng/mL质量浓度范围的线性方程为Y=0.0586X+0.00726, r=0.9965; AME在0.20~10.0 ng/mL质量浓度范围的线性方程为Y=0.0759X-0.00106, r=0.9995; AOH在2.50~50.0 ng/mL质量浓度范围的线性方程为Y=0.0734X-0.0528, r=0.9997。TeA、TEN、AME和AOH的检出限为2.00、0.10、0.10和1.00 μg/kg。分析过程通过加标回收实验和平行双样控制分析质量, 每10个样做一个平行样, 每批样品做一个空白样和样品加标。加标回收实验的回收率为93.6%~107.5%, 平行双样的RSDs小于10%。
2.2 陕西省小麦中镰刀菌毒素和交链孢毒素污染状况
陕西省小麦被镰刀菌毒素DON及其衍生物、NIV、ZEN和交链孢毒素TeA、TEN、AME污染。检出率最高为TeA和TEN, 其次是AME。阳性平均值最高的是DON, 其次是TeA(表2)。小麦中镰刀菌毒素DON、3-AcDON、15-AcDON、NIV和ZEN的检出率分别为83.3%、5.00%、10.0%、11.6%和8.33%, 阳性污染水平(平均含量评价)分别为600、15.6、19.7、92.3和8.65 μg/kg。DON最大浓度达到3210 μg/kg, 超我国小麦DON的限量标准(1000 μg/kg)。
小麦样品全部检出交链孢霉毒素。TeA、TEN和AME的检出率为100.0%、100.0%和98.3%, 阳性污染水平分别为128、25.6和29.2 μg/kg(表2)。TeA的含量主要集中在2.00~500 μg/kg, 占比为96.6%。TEN的含量主要集中在0.10~50.00 μg/kg, 占比为91.6%。
2.3 陕西省小麦粉中镰刀菌毒素和交链孢毒素污染状况
陕西省小麦粉被镰刀菌毒素DON和交链孢毒素TeA、TEN、AME污染。检出率最高为TeA, 其次是TEN。阳性平均值最高的是DON, 其次是TeA(表3)。小麦粉只有镰刀菌毒素DON检出, 检出率为87.5%, 阳性污染水平为267 μg/kg, 最大浓度947 μg/kg, 超欧盟限量标准, 但低于我国限量标准。小麦粉中交链孢霉毒素TeA、TEN和AME的检出率为96.2%、88.7%和63.7%, 阳性污染水平分别为44.3、5.04和0.63 μg/kg。
2.4 小麦和小麦粉中镰刀菌毒素和交链孢毒素联合污染情况及相关性分析
通过对阳性样品的统计分析, 小麦和小麦粉样品同时被镰刀菌毒素和交链孢毒素污染, 主要以DON、TeA、TEN和其他毒素的混合污染最为常见。其中被2种、3种、4种和5种毒素同时污染的样品分别占总样品的14.3% (20/140)、23.6% (33/140)、45.7% (64/140)和16.4% (23/140)。本研究对小麦和小麦粉中镰刀菌毒素和交链孢毒素含量进行相关性分析, P<0.05为差异有统计学意义。由于AOH在所有样本中均未检出, ZEN只有一份样品检出, 因此只含有7种毒素的相关性分析。由表4可以看出, 正相关性最强的是DON与15-AcDON (r=0.825, P<0.01)、TeA与TEN (r=0.805, P<0.01), 其次是3-AcDON与15-AcDON (r=0.572, P<0.01)、3-AcDON与DON (r=0.554, P<0.01), 其他毒素之间是弱相关(r<0.4, P<0.05)或无相关性(P>0.05)。上述结果表明镰刀菌毒素和交链孢霉毒素之间的污染相关性弱; 被DON污染的样品, 很有可能伴随着3-AcDON、15-AcDON的污染; 被TeA污染的样品, 大概率伴随TEN的污染。
2.5 小麦粉的镰刀菌毒素和交链孢毒素膳食暴露风险评估
参考第五次中国总膳食研究中陕西省12类食品样品聚类后食物品种及消费量[26], 陕西省居民平均每日小麦粉消费量(挂面、馒头、油饼和蛋糕消费量加和)为215.69 g。小麦粉中DON、TeA、TEN、AME的膳食暴露量分别为959.8、159.2、18.1和2.30 ng/(kg·bw·d)。镰刀菌毒素DON的TDI值为1300 ng/(kg·bw·d)[27]。镰刀菌毒素DON的膳食暴露量959.8 ng/(kg·bw·d)小于TDI值。按照TTC决策树, 由于交链孢毒素AME具有遗传毒性, 其TTC值为2.50 ng/(kg·bw·d)[28], 交链孢毒素AME的膳食暴露量2.30 ng/(kg·bw·d)小于其TTC值。按照TTC决策树中Cramer的化合物分级(根据物质化学结构不同将其分为Ⅰ、Ⅱ、Ⅲ类), TeA和TEN属于第Ⅲ类化合物, 其TTC值为1500 ng/(kg bw·d)[28]。交链孢毒素TeA的膳食暴露量159.2 ng/(kg·bw·d)小于其TTC值, 约为TTC值的11%。交链孢毒素TEN的膳食暴露量18.1 ng/(kg·bw·d)小于其TTC值, 约为TTC值的1.2%。结果表明, 本年度通过小麦粉DON、TeA、TEN、AME膳食暴露对消费者健康影响风险较小。
3 讨论与结论
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本研究结果表明,2022—2024年陕西省小麦和小麦粉都受到镰刀菌毒素不同程度的污染。小麦和小麦粉中检出DON、3-AcDON、15-AcDON、NIV和ZEN, DON与15-AcDON含量表现出非常强相关性。2022—2024年陕西省小麦粉中DON的检出率和超标率分别为87.5%和0.0%,较胡佳薇等[29]2013—2016年陕西省小麦粉及其制品的检出率86.9%和超标率6.70%, 超标率显著下降, 这是因为GB 2715—2016《食品安全国家标准 粮食》要求小麦中霉变粒小于等于2%, 小麦粉DON项目列入出厂检验指标。小麦粉中镰刀菌毒素DON的膳食暴露量小于TDI值, 处于可接受的风险范围内。
陕西省小麦和小麦粉均受到交链孢毒素不同程度的污染。小麦和小麦粉中检出TeA、TEN和AME, TeA与TEN含量表现出非常强的相关性, 与赵凯[30]研究结果相符。陕西省小麦粉中TeA、TEN、AOH和AME的平均浓度分别为44.3、5.04、0.63和0 μg/kg。何玲等[31]对四川省市售小麦及其制品中交链孢霉毒素进行检测, TeA、TEN、AOH和AME的平均浓度分别为27.2、4.78、0.75和0.57 μg/kg。陈蓓等[32]对江苏省内小麦粉中4种交链孢霉毒素进行检测, TeA、TEN、AOH和AME的平均浓度分别为56.1、6.7、2.0和1.2 μg/kg。由此可知, 小麦粉中TeA污染最严重, 其次是TEN, AOH和AME污染水平较低。小麦粉中交链孢毒素TeA、TEN、AME的膳食暴露量小于TTC值, 对消费者健康影响的风险较小。我国关于交链孢霉毒素污染谷物的研究相对较少, 而且目前世界范围内都没有制定交链孢霉毒素的限量标准, 因此我国应多开展交链孢霉毒素的调查研究, 收集污染数据, 加快制定交链孢霉毒素的限量标准, 保障我国食品安全。
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2025年第16卷第16期
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20250529001
  • 接收时间：2025-05-29
  • 首发时间：2026-01-13
  • 出版时间：2025-08-25
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  • 收稿日期：2025-05-29
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    陕西省疾病预防控制中心, 西安 710054

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* 赵迪(1987—), 女, 硕士, 助理研究员, 主要研究方向为食品理化检验。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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