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Article(id=1217529311372952232, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217529305693864468, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20250119001, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1737216000000, receivedDateStr=2025-01-19, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1768211208432, onlineDateStr=2026-01-12, pubDate=1752508800000, pubDateStr=2025-07-15, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1768211208432, onlineIssueDateStr=2026-01-12, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1768211208432, creator=13701087609, updateTime=1768211208432, updator=13701087609, issue=Issue{id=1217529305693864468, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='13', 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=null, createTime=1768211207077, creator=13701087609, updateTime=1768212057891, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1217532874337730593, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217529305693864468, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1217532874337730594, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217529305693864468, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=248, endPage=254, ext={EN=ArticleExt(id=1217529311851102916, articleId=1217529311372952232, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Research on the false positive interference mechanism of thebaine in the spices of hot pot base materials, columnId=1151895321388347923, journalTitle=Journal of Food Safety & Quality, columnName=Food Analysis and Detection, runingTitle=null, highlight=null, articleAbstract=

Objective To investigate false positive interference from spices in hot pot base materials during the detection of thebaine using mass spectrometry, identify interfering matrix components, and optimize analytical methods. Methods The 62 kinds of commonly used spices in hot pot bases were collected. The false positive issues screened by BJS 201802 Determination method of morphine, codeine, papaverine, noscapine and thebaine in food were further analyzed by Fourier transform ion cyclotron resonance mass spectrometry combined with positive pressure electrospray ionization full mass spectrometry scanning. The potential interfering substances were locked through ion fragment analysis and verified. Results The results showed that the detection found interference peaks with retention times similar to those of thebaine in the extracts of bay leaves and pepper, which could lead to false positive results. The molecular weight of the interfering substance was 311.3812 ([M+H]+), with a deviation of less than 2 ppm from the theoretical value of thebaine (311.375), suggesting that it was an isomer. Through the detection of the suspected interfering substance, it was verified that Launobine and Pisatin had no interfering activity. Conclusion The alkaloid substances in spices have significant interference with the detection of thebaine. It is suggested to improve the specificity and accuracy of the detection by optimizing the mass spectrometry conditions, introducing nuclear magnetic resonance technology and perfecting the pretreatment process to avoid false positive misjudgment.

, correspAuthors=Si-Yu JIANG, 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=Lin-Hua LIAO, Si-Yu JIANG, Ze-Rong JIN, Li YANG, Yan-Kang YANG), CN=ArticleExt(id=1217529314791310151, articleId=1217529311372952232, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=火锅底料香辛料中蒂巴因假阳性干扰机制研究, 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 排查火锅底料中香辛料对质谱检测蒂巴因的假阳性干扰, 明确其干扰基质并优化检测方法。方法 收集62种火锅底料中常用香辛料, 通过BJS 201802《食品中吗啡、可待因、罂粟碱、那可丁和蒂巴因的测定方法》筛查的假阳性问题, 进一步使用傅里叶变换离子回旋共振质谱法结合正压电喷雾电离全质谱扫描分析, 通过离子碎片解析锁定潜在干扰物, 并进行验证。结果 检测发现月桂叶与荜拨提取物中存在与蒂巴因保留时间相近的干扰峰, 导致易被误判为阳性。其中干扰物分子量为311.381([M+H]+), 与蒂巴因理论值(311.375)偏差<2 ppm, 推测其为同分异构体。通过对推测的干扰物检测, 验证Launobine与Pisatin无干扰活性。结论 香辛料中生物碱类物质对蒂巴因检测存在显著干扰, 建议通过优化质谱条件、引入核磁共振技术及完善前处理流程, 提升检测特异性与准确性, 避免假阳性误判。

, correspAuthors=蒋思雨, authorNote=null, correspAuthorsNote=
*蒋思雨(1997—), 女, 硕士, 助理工程师, 主要研究方向为食品安全检测。E-mail:
, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=o0T+/RWiaD1cpO2wqDGXCg==, magXml=K+Iey1Ia/nOpDmBjr+dmhA==, pdfUrl=null, pdf=q3wVzqfCWmt55GyCjzXELQ==, pdfFileSize=1084997, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=3kK8KprTyJ5a6iym2qdPRQ==, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=2OsuZ5R/dtxEuVk4OWzkEg==, mapNumber=null, authorCompany=null, fund=null, authors=

廖林华(1995—), 女, 助理工程师, 主要研究方向为食品安全检测。E-mail:

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廖林华(1995—), 女, 助理工程师, 主要研究方向为食品安全检测。E-mail:

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廖林华(1995—), 女, 助理工程师, 主要研究方向为食品安全检测。E-mail:

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Determination of papaverine in hotpot seasoning by double column separation-gas chromatography[J]. Chinese Journal of Health Laboratory Technology, 2015, 14: 2296-2298., articleTitle=Determination of papaverine in hotpot seasoning by double column separation-gas chromatography, refAbstract=null), Reference(id=1217901262956319698, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, doi=null, pmid=null, pmcid=null, year=2008, volume=65, issue=4, pageStart=403, pageEnd=408, url=null, language=null, rfNumber=[29], rfOrder=48, authorNames=KASPEREK R, journalName=Acta Poloniae Pharmaceutica, refType=null, unstructuredReference=KASPEREK R. Determination of diclofenac sodium and papaverine hydrochloride in tablets by HPLC method[J]. 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(Papaveraceae), refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1217901246598533215, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, xref=1, ext=[AuthorCompanyExt(id=1217901246611116130, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, companyId=1217901246598533215, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 Sichuan AIF Testing Co., Ltd., Chengdu 611130, China), AuthorCompanyExt(id=1217901246632087650, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, companyId=1217901246598533215, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 四川敏恩检测技术有限公司, 成都 611130)]), AuthorCompany(id=1217901246724362342, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, xref=2, ext=[AuthorCompanyExt(id=1217901246736945256, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, companyId=1217901246724362342, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2 Chengdu SNS Biotechnology Co., Ltd., Chengdu 611130, China), AuthorCompanyExt(id=1217901246745333868, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, companyId=1217901246724362342, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2 成都圣恩生物科技股份有限公司, 成都 611130)])], figs=[ArticleFig(id=1217901251002552668, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, language=EN, label=Fig.1, caption=Comparison of the spectra of Laurus nobilis, Piper longum and thebaine, figureFileSmall=xgebA9ZGzXkvXA1dTcCTFg==, figureFileBig=3WmmUhzIN3rOWlDNkbbN1g==, tableContent=null), ArticleFig(id=1217901251082244452, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, language=CN, label=图1, caption=月桂叶、荜拨与蒂巴因谱图对比, figureFileSmall=xgebA9ZGzXkvXA1dTcCTFg==, figureFileBig=3WmmUhzIN3rOWlDNkbbN1g==, tableContent=null), ArticleFig(id=1217901251220656501, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, language=EN, label=Fig.2, caption=Comparison of flight time mass spectrometry ion images of Laurus nobilis, Piper longum and thebaine, figureFileSmall=r5nrWIPY6txouLvrlmOExw==, figureFileBig=qo561srUpegl2vySA976+Q==, tableContent=null), ArticleFig(id=1217901251329708413, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, language=CN, label=图2, caption=月桂叶、荜拨与蒂巴因飞行质谱离子图对比, figureFileSmall=r5nrWIPY6txouLvrlmOExw==, figureFileBig=qo561srUpegl2vySA976+Q==, tableContent=null), ArticleFig(id=1217901251522646406, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, language=EN, label=Fig.3, caption=Chemical formula of thebaine, figureFileSmall=ZqBT2Wmn3nDa3FxcJx3MCw==, figureFileBig=S/apeyZSExF0gfGYoVNAWA==, tableContent=null), ArticleFig(id=1217901251690418575, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, language=CN, label=图3, caption=蒂巴因化学式, figureFileSmall=ZqBT2Wmn3nDa3FxcJx3MCw==, figureFileBig=S/apeyZSExF0gfGYoVNAWA==, tableContent=null), ArticleFig(id=1217901251782693272, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, language=EN, label=Fig.4, caption=Chemical formula of suspected interferents, figureFileSmall=Qa9BOUi0GBoMv1HIQnUL2w==, figureFileBig=rwf8bhrHmGM9cIwa/0JZdg==, tableContent=null), ArticleFig(id=1217901251916911006, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, language=CN, label=图4, caption=疑似干扰物化学式, figureFileSmall=Qa9BOUi0GBoMv1HIQnUL2w==, figureFileBig=rwf8bhrHmGM9cIwa/0JZdg==, tableContent=null), ArticleFig(id=1217901252021768615, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, language=EN, label=Table 1, caption=

Test results of spices

, figureFileSmall=null, figureFileBig=null, tableContent=
标准名称/目录 序号 样品名称 产地 蒂巴因 标准名称/目录 序号 样品名称 产地 蒂巴因
卫健委公布的药食两用目录与GB/T 12729.1—2008《香辛料和调味品 名称》中共有香辛料 1 八角 广西 - GB/T 12729.1—2008中独有香辛料 32 白胡椒(粉A2) 印尼 -
2 桂皮(去皮桂丝) 广西 - 33 子弹椒 河南 -
3 山奈 广西 - 34 子弹椒(节) 河南 -
4 草果 云南 - 35 满天星(节) 贵州 -
5 砂仁 云南 - 36 印度椒 印尼 -
6 丁香 印尼 - 37 印度椒(节) 印尼 -
7 小茴香 甘肃 - 38 皱椒 新疆 -
8 荜拨 印尼 疑似检出 39 石柱红辣椒 河南 -
9 红花椒(颗粒) 甘肃 - 40 米粉椒 新疆 -
10 青花椒(颗粒) 云南 - 41 北京红辣椒(节) 内蒙古 -
11 干姜(片) 云南 - 42 二荆条辣椒(节) 新疆 -
12 姜(粉) 山东 - 43 829辣椒(节) 甘肃 -
13 甘草 甘肃 - 44 内黄新一代辣椒 河南 -
14 黑胡椒 海南 - 45 三樱8号辣椒 河南 -
15 姜黄(粉) 印度 - 46 香茅 云南 -
16 高良姜 广东 - 47 枯茗(孜然) 新疆 -
17 肉豆蔻 云南 - 48 百里香 印尼 -
18 当归(碎) 广西 - 49 迷迭香 印度尼西亚 -
卫健委公布的药食两用目录独中香辛料 19 橘皮 湖北 - 50 黄洋葱(粉) 甘肃 -
20 山楂 河北 - 51 香葱(粉) 兴化 -
21 罗汉果 广西 - 52 葱白(粉) 山东 -
22 栀子 江西 - 53 红葱(粉) 甘肃 -
23 紫苏 云南 - 54 蒜(粉) 山东 -
24 薏仁(粉) 贵州 - 其他香辛料 55 咖喱调味粉 江苏泰州
25 白芷 遂宁 - 56 酸辣粉辣椒面 四川
26 广藿香 / - 57 日式咖喱粉 江苏泰州
27 芫荽(籽) 湖北 - 58 十三香 驻马店
GB/T 12729.1—2008中独有香辛料 28 豆蔻 印尼 - 59 油桂粉 越南 -
29 月桂(叶) 土耳其 疑似检出 60 台式五香粉 商丘 -
30 白胡椒 海南 - 61 海带粉 兴华 -
31 白胡椒(粉) 海南 - 62 甜椒粉 新疆 -
), ArticleFig(id=1217901252147597744, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, language=CN, label=表1, caption=

香辛料检测结果

, figureFileSmall=null, figureFileBig=null, tableContent=
标准名称/目录 序号 样品名称 产地 蒂巴因 标准名称/目录 序号 样品名称 产地 蒂巴因
卫健委公布的药食两用目录与GB/T 12729.1—2008《香辛料和调味品 名称》中共有香辛料 1 八角 广西 - GB/T 12729.1—2008中独有香辛料 32 白胡椒(粉A2) 印尼 -
2 桂皮(去皮桂丝) 广西 - 33 子弹椒 河南 -
3 山奈 广西 - 34 子弹椒(节) 河南 -
4 草果 云南 - 35 满天星(节) 贵州 -
5 砂仁 云南 - 36 印度椒 印尼 -
6 丁香 印尼 - 37 印度椒(节) 印尼 -
7 小茴香 甘肃 - 38 皱椒 新疆 -
8 荜拨 印尼 疑似检出 39 石柱红辣椒 河南 -
9 红花椒(颗粒) 甘肃 - 40 米粉椒 新疆 -
10 青花椒(颗粒) 云南 - 41 北京红辣椒(节) 内蒙古 -
11 干姜(片) 云南 - 42 二荆条辣椒(节) 新疆 -
12 姜(粉) 山东 - 43 829辣椒(节) 甘肃 -
13 甘草 甘肃 - 44 内黄新一代辣椒 河南 -
14 黑胡椒 海南 - 45 三樱8号辣椒 河南 -
15 姜黄(粉) 印度 - 46 香茅 云南 -
16 高良姜 广东 - 47 枯茗(孜然) 新疆 -
17 肉豆蔻 云南 - 48 百里香 印尼 -
18 当归(碎) 广西 - 49 迷迭香 印度尼西亚 -
卫健委公布的药食两用目录独中香辛料 19 橘皮 湖北 - 50 黄洋葱(粉) 甘肃 -
20 山楂 河北 - 51 香葱(粉) 兴化 -
21 罗汉果 广西 - 52 葱白(粉) 山东 -
22 栀子 江西 - 53 红葱(粉) 甘肃 -
23 紫苏 云南 - 54 蒜(粉) 山东 -
24 薏仁(粉) 贵州 - 其他香辛料 55 咖喱调味粉 江苏泰州
25 白芷 遂宁 - 56 酸辣粉辣椒面 四川
26 广藿香 / - 57 日式咖喱粉 江苏泰州
27 芫荽(籽) 湖北 - 58 十三香 驻马店
GB/T 12729.1—2008中独有香辛料 28 豆蔻 印尼 - 59 油桂粉 越南 -
29 月桂(叶) 土耳其 疑似检出 60 台式五香粉 商丘 -
30 白胡椒 海南 - 61 海带粉 兴华 -
31 白胡椒(粉) 海南 - 62 甜椒粉 新疆 -
), ArticleFig(id=1217901252386673091, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, language=EN, label=Table 2, caption=

Table of similar chemical constituents of laurel leaves, canola and tibacin

, figureFileSmall=null, figureFileBig=null, tableContent=
来源 化学成分英文名称 化学成分中文名称 CAS号 分子式 分子量
蒂巴因 thebaine 蒂巴因 115-37-7 C19H21NO3 311.375
782491-54-7 C19H18D3NO3 314.393
月桂叶 actinodaphnine 黄肉楠碱 517-69-1 C18H17NO4 311.332
launobine 无根藤次碱 20497-21-6 C18H17NO4 311.332
荜拨 pisatin 豌豆素 20186-22-5 C17H14NO6 314.289
/ nalorphine 烯丙吗啡 62-67-9 C19H21NO3 311.381
/ isothebaine 异蒂巴因 568-21-8 C19H21NO3 311.381
/ pronuciferine 原荷叶碱 2128-60-1 C19H21NO3 311.381
), ArticleFig(id=1217901252495725002, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, language=CN, label=表2, caption=

月桂叶、荜拨与蒂巴因相近化学成分表

, figureFileSmall=null, figureFileBig=null, tableContent=
来源 化学成分英文名称 化学成分中文名称 CAS号 分子式 分子量
蒂巴因 thebaine 蒂巴因 115-37-7 C19H21NO3 311.375
782491-54-7 C19H18D3NO3 314.393
月桂叶 actinodaphnine 黄肉楠碱 517-69-1 C18H17NO4 311.332
launobine 无根藤次碱 20497-21-6 C18H17NO4 311.332
荜拨 pisatin 豌豆素 20186-22-5 C17H14NO6 314.289
/ nalorphine 烯丙吗啡 62-67-9 C19H21NO3 311.381
/ isothebaine 异蒂巴因 568-21-8 C19H21NO3 311.381
/ pronuciferine 原荷叶碱 2128-60-1 C19H21NO3 311.381
), ArticleFig(id=1217901253833707991, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, language=EN, label=Table 3, caption=

Detection results of selected interferences

, figureFileSmall=null, figureFileBig=null, tableContent=
来源 英文名称 CAS号 分子量 蒂巴因
检测结果
月桂叶 Launobine 20497-21-6 311.332 未检出
荜拨 Pisatin 20186-22-5 314.289 未检出
), ArticleFig(id=1217901253963731427, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529311372952232, language=CN, label=表3, caption=

部分干扰物检测结果

, figureFileSmall=null, figureFileBig=null, tableContent=
来源 英文名称 CAS号 分子量 蒂巴因
检测结果
月桂叶 Launobine 20497-21-6 311.332 未检出
荜拨 Pisatin 20186-22-5 314.289 未检出
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火锅底料香辛料中蒂巴因假阳性干扰机制研究
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廖林华 1 , 蒋思雨 1, * , 靳泽荣 1 , 杨莉 1 , 杨延康 2
食品安全质量检测学报 | 食品分析与检测 2025,16(13): 248-254
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食品安全质量检测学报 | 食品分析与检测 2025, 16(13): 248-254
火锅底料香辛料中蒂巴因假阳性干扰机制研究
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廖林华1 , 蒋思雨1, * , 靳泽荣1, 杨莉1, 杨延康2
作者信息
  • 1 四川敏恩检测技术有限公司, 成都 611130
  • 2 成都圣恩生物科技股份有限公司, 成都 611130

    • 廖林华(1995—), 女, 助理工程师, 主要研究方向为食品安全检测。E-mail:

通讯作者:

*蒋思雨(1997—), 女, 硕士, 助理工程师, 主要研究方向为食品安全检测。E-mail:
Research on the false positive interference mechanism of thebaine in the spices of hot pot base materials
Lin-Hua LIAO1 , Si-Yu JIANG1, * , Ze-Rong JIN1, Li YANG1, Yan-Kang YANG2
Affiliations
  • 1 Sichuan AIF Testing Co., Ltd., Chengdu 611130, China
  • 2 Chengdu SNS Biotechnology Co., Ltd., Chengdu 611130, China
出版时间: 2025-07-15 doi: 10.19812/j.cnki.jfsq11-5956/ts.20250119001
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摘要
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目的 排查火锅底料中香辛料对质谱检测蒂巴因的假阳性干扰, 明确其干扰基质并优化检测方法。方法 收集62种火锅底料中常用香辛料, 通过BJS 201802《食品中吗啡、可待因、罂粟碱、那可丁和蒂巴因的测定方法》筛查的假阳性问题, 进一步使用傅里叶变换离子回旋共振质谱法结合正压电喷雾电离全质谱扫描分析, 通过离子碎片解析锁定潜在干扰物, 并进行验证。结果 检测发现月桂叶与荜拨提取物中存在与蒂巴因保留时间相近的干扰峰, 导致易被误判为阳性。其中干扰物分子量为311.381([M+H]+), 与蒂巴因理论值(311.375)偏差<2 ppm, 推测其为同分异构体。通过对推测的干扰物检测, 验证Launobine与Pisatin无干扰活性。结论 香辛料中生物碱类物质对蒂巴因检测存在显著干扰, 建议通过优化质谱条件、引入核磁共振技术及完善前处理流程, 提升检测特异性与准确性, 避免假阳性误判。

罂粟碱  /  火锅底料  /  香辛料  /  假阳性

Objective To investigate false positive interference from spices in hot pot base materials during the detection of thebaine using mass spectrometry, identify interfering matrix components, and optimize analytical methods. Methods The 62 kinds of commonly used spices in hot pot bases were collected. The false positive issues screened by BJS 201802 Determination method of morphine, codeine, papaverine, noscapine and thebaine in food were further analyzed by Fourier transform ion cyclotron resonance mass spectrometry combined with positive pressure electrospray ionization full mass spectrometry scanning. The potential interfering substances were locked through ion fragment analysis and verified. Results The results showed that the detection found interference peaks with retention times similar to those of thebaine in the extracts of bay leaves and pepper, which could lead to false positive results. The molecular weight of the interfering substance was 311.3812 ([M+H]+), with a deviation of less than 2 ppm from the theoretical value of thebaine (311.375), suggesting that it was an isomer. Through the detection of the suspected interfering substance, it was verified that Launobine and Pisatin had no interfering activity. Conclusion The alkaloid substances in spices have significant interference with the detection of thebaine. It is suggested to improve the specificity and accuracy of the detection by optimizing the mass spectrometry conditions, introducing nuclear magnetic resonance technology and perfecting the pretreatment process to avoid false positive misjudgment.

papaverine  /  hot pot base materials  /  spices  /  false positives interference
廖林华, 蒋思雨, 靳泽荣, 杨莉, 杨延康. 火锅底料香辛料中蒂巴因假阳性干扰机制研究. 食品安全质量检测学报, 2025 , 16 (13) : 248 -254 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250119001
Lin-Hua LIAO, Si-Yu JIANG, Ze-Rong JIN, Li YANG, Yan-Kang YANG. Research on the false positive interference mechanism of thebaine in the spices of hot pot base materials[J]. Journal of Food Safety & Quality, 2025 , 16 (13) : 248 -254 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250119001
正文
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0 引言
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火锅作为中华饮食文化的代表性载体, 兼具烹饪艺术与社会功能, 其全球化的普及也带来了食品安全监管的新挑战[1]。近年来, 不法商贩为谋取利益, 在火锅底料中非法添加罂粟壳等违禁物质的现象频发。例如, 2024年成都市青羊区某兔火锅店[2]、2019年郫都区陈华火锅店及2018年峨眉山市念念有鱼自助火锅店均被检出含有罂粟碱成分[3], 凸显了这一问题的严重性。
蒂巴因是罂粟壳中最主要的活性生物碱之一, 其化学结构与吗啡类似, 可通过抑制中枢神经系统产生欣快感与成瘾性[4-6]。研究表明, 长期低剂量摄入蒂巴因[<0.1 mg/(kg· 日]即可引发依赖性, 过量摄入可能导致呼吸抑制、心律失常甚至死亡[7]。基于其成瘾性与公共卫生风险, 被列为严格管控的麻醉药品(联合国《1961年麻醉品单一公约》)。我国《食品安全法》及《食品中可能违法添加的非食用物质和易滥用的食品添加剂名单》(2009版)明令禁止在食品中添加罂粟壳及其衍生物, 并将其归类为“可能违法添加的非食用物质”[5]。尽管如此, 罂粟壳因其增香提味特性仍被部分商家违规使用, 而现有检测技术的局限性加剧了监管难度。当前, 针对火锅底料中罂粟碱的检测主要依赖高效液相色谱-串联质谱(high performance liquid chromatography-mass spectrometry, HPLC-MS/MS)技术, 如BJS 201802《食品中吗啡、可待因、罂粟碱、那可丁和蒂巴因的测定》方法。然而, 该方法在复杂基质中易受香辛料中内源性生物碱干扰。孙姗姗等[6]研究发现, 月桂叶与荜拨提取物中存在与蒂巴因保留时间相近的干扰峰, 且碎片离子谱相似度高, 导致假阳性率高达15%。
鉴于此, 本研究基于上述背景, 通过系统筛查62种火锅底料常用香辛料, 揭示其与蒂巴因检测的关联性干扰规律。结合HPLC-MS/MS与傅里叶变换离子回旋共振质谱法, 探究假阳性干扰机制, 为行业提供有效的检测方法和策略, 以保障消费者的饮食安全。
1 材料与方法
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1.1 材料
本研究选用火锅底料中常用的香辛料, 包含卫健委公布的药食两用目录中香辛料: 橘皮、山楂、罗汉果、栀子、紫苏、薏苡仁(粉)、白芷、广藿香、芫荽(籽); GB/T 12729.1—2008《香辛料和调味品 名称》中有香辛料: 豆蔻、月桂(叶)、白胡椒(白胡椒粉、白胡椒粉A2)、辣椒(子弹椒节、子弹椒、满天星节、印度椒节、印度椒、皱椒、石柱红辣椒、米粉椒、北京红辣椒、二荆条辣椒、829辣椒节、内黄新一代辣椒、三樱8号辣椒)、香茅、枯茗(孜然)、百里香、迷迭香、黄洋葱(粉)、葱(香葱粉、葱白粉、红葱粉)、蒜(粉); 卫健委公布的药食两用目录与GB/T 12729.1—2008中共有香辛料: 八角、肉桂(去皮桂丝)、山奈、草果、砂仁、丁香、小茴香、荜拨、红花椒(颗粒)、青花椒(颗粒)、干姜(片)、甘草、黑胡椒、姜黄(粉)、高良姜、肉豆蔻、当归(碎); 其他香辛料: 咖喱调味粉、酸辣粉辣椒面、十三香、日式咖喱粉、油桂粉、台式五香粉、甜椒粉、海带粉, 所使用的香辛料均来自成都圣恩生物科技股份有限公司。
1.2 仪器与试剂
1290II-6460高效液相色谱-三重四极杆串联质谱仪(带电喷雾离子源)、HILIC色谱柱(2.1 mm×100 mm, 1.7 μm) (美国安捷伦公司); SB25-12DTDN超声波清洗机(宁波新芝生物科技股份有限公司); ME204电子分析天平(感量为0.1 mg, 上海梅特勒-托利多仪器有限公司); HR/T20MM立式高速冷冻离心机(湖南赫西仪器装备有限公司)。
蒂巴因标准物质(质量浓度10 μg/mL, 坛墨质检科技股份有限公司); 乙腈、甲醇、甲酸(质谱级, 美国Fisher公司); 甲酸铵(质谱级, 天津市科密欧化学试剂有限公司); 无水硫酸镁、无水乙酸钠、氢氧化钠(分析纯, 成都诺尔施科技有限公司)。
1.3 实验方法
1.3.1 仪器条件
色谱条件: HILIC色谱柱(2.1 mm×100 mm, 1.7 μm); 流动相: A: 0.1%甲酸-10 mm甲酸铵5%乙腈水溶液, B: 0.1%甲酸乙腈溶液, 梯度洗脱程序: 0 min A相95%, 1.0 min A相95%, 6.0 min A相85%, 6.5 min A相60%, 8.0 min A相60%, 8.1 min A相95%, 12.0 min A相95%; 流速: 0.3 mL/min; 柱温: 40 ℃; 质谱条件: 离子化模式: 电喷雾正离子模式: 扫描模式: 多离子反应监测; 离子源温度: 120 ℃; 锥孔电压: 25 V; 毛细管电压: 3.5 kV; 锥孔气流量: 150 L/h; 脱溶剂温度: 400 ℃; 脱溶剂气流量: 800 L/h; 定性离子对: 定量离子58.2 m/z, 定性离子66.1 m/z。
1.3.2 前处理方法
参照BJS 201802: 将所有香辛料样品研磨成粉状, 制备量大于50 g, 混匀好的样品分为两份, 分别作为试样(>20 g)和留样(>20 g), 装于洁净聚四氟乙烯离心管中, 密封并标记, 常温保存。
称取2 g样品于50 mL离心管内, 加5 mL 0.1 mol/L盐酸溶液涡旋30 s, 加入15 mL乙腈, 涡旋混匀1 min, 40 kHz超声30 min。加入6 g无水硫酸镁, 1.5 g无水乙酸钠。涡旋2 min, 5000 r/min 离心5 min。移取上清液, 0.22 μm滤膜过滤, 取滤液待测。
1.3.3 标准溶液配制
标准储备液(100 ng/mL): 准确吸取0.1 mL混合标准物质至10 mL容量瓶中, 用乙腈定容至刻度。现配现用。
标准应用液(10 ng/mL): 准确吸取1 mL混合标准物质至10 mL容量瓶中, 用乙腈定容至刻度。现配现用。
标准工作液: 精密量取混合标准中间液适量, 加乙腈配制系列混合标准工作液, 质量浓度分别为0.5、1.0、1.5、5.0、10.0、20.0、30.0、50.0 ng/mL。现配现用。
1.3.4 方法学考察
(1)标准曲线及相关系数
参照BJS 201802与GB/T 27417—2017《合格评定化学分析方法确认和验证指南》, 采用标准曲线法定量, 并至少具有6个校准点, 根据方法最低检出限制定不同浓度的标准曲线方程, 拟定标准曲线溶液质量浓度为: 0.5、1.0、1.5、5.0、10.0、20.0、30.0、50.0 ng/mL, 用空白辣椒红样品基质配制混合标准溶液, 通过绘制峰面积与浓度的关系, 考察线性方程和相关系数(r2)。用不同试剂及空白提取液分别配制, 验证其标准曲线拟合度及相关系数。
(2)准确性
参照GB/T 27404—2008《实验室质量控制规范 食品理化检测》、GB/T 27417—2017及GB/T 32465—2015《化学分析方法验证确认和内部质量控制要求》, 对样品进行3个不同质量浓度(1.5、10.0、30.0 ng/mL)的加标实验, 每个质量浓度重复测定6次, 验证其准确性。
1.3.5 干扰物结果鉴定及分析
将待测样品采集到的高分辨数据导入定性筛查软件, 利用软件通过对样品中色谱峰进行一级同位素拟合匹配分析确定其分子式和加合方式, 再通过该化合物二级碎片离子模拟各对应化学基团, 再依据其裂解规律推断出化合物结构式, 最后依据化合物分子式在ChemSpider 官方网站搜索, 结合其化学结构式鉴定该干扰物[8-11]。
1.4 数据处理
实验结果采用Excel 2017表格进行数据的记录和统计, 采用平均值±标准偏差进行计算, 采用Origin Pro 8.5软件进行作图分析。
2 结果与分析
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2.1 方法学考察
2.1.1 标准曲线与相关系数
在质量浓度范围内, 以各组分的峰面积为纵坐标, 质量浓度为横坐标(X, ng/mL), 响应值为纵坐标(Y)绘制蒂巴因的混合标准曲线, 计算出蒂巴因响应的线性回归方程为Y=1715.67 X+743.91, 相关系数(r2)在0.9968, 表示在0.5~50.0 ng/mL质量浓度范围内蒂巴因呈现出良好的线性关系。
2.1.2 准确性
通过添加1.5、10.0、30.0 ng/mL质量浓度蒂巴因, 回收率为96.2%~100.9%, 相对标准偏差在2.1%~4.1%。符合GB/T 27404—2008标准中表F.1的相关规定。对于含量低于0.1 mg/kg的被测组分, 回收率应在60%至120%之间; 而对于含量在0.1~1.0 mg/kg之间的被测组分, 回收率应在80%至110%之间。实验结果表明, 该方法回收率高于标准要求上限, 表明该方法准确性满足实验要求。
2.2 样品测定结果
如表1所示, 对62种不同种类香辛料进行检测, 按照BJS 201802方法进行处理, 高效液相色谱-质谱法进行分析。实验发现月桂叶和荜拨2种香辛料有疑似罂粟碱成分检出, 这与孙姗姗等[6]报道相似。对同种香辛料扩大至5批次检测, 结果相同, 但这些香料与罂粟壳并非同属植物, 可能存在其他干扰原因。
2.3 干扰物筛查分析
2.3.1 离子丰度比考察
蒂巴因是一种有机化合物, 化学式为C19H21NO3, 是一种异喹啉生物碱。其特定的化学结构, 包括特定的官能团和骨架, 使得蒂巴因在质谱等分析技术中具有独特的信号特征[12-13]。然而, 某些香辛料中的天然成分, 如生物碱、酚类化合物等, 也可能具有与蒂巴因相似的化学结构特征。这些相似的化学结构可能导致在质谱图上产生重叠或相似的峰形, 从而干扰蒂巴因的准确检测[14]。
按照BJS 201802方法检验时发现, 蒂巴因标准物质色谱峰保留时间为4.454 min, 月桂叶与荜拨样品色谱峰保留时间为4.454 min、4.620 min, 保留时间最大相差0.166 min。依据BJS 201802方法的规定, 在正离子扫描模式下, 母离子为312.2 (m/z), 子离子58.2 (m/z)为定量离子, 子离子266.1 (m/z)为定性离子(图1), 通过提取子离子峰面积比较发现, 离子丰度比与标准相比, 并没有超出范围。因此, 对存在假阳性问题的香辛料与标准品进行对比, 发现其保留时间与标准品出峰时间相近且存在相同子离子, 但定性离子丰度比与标准品差异较大[15-17]。根据质谱端采集原理, 这可能是因为该香辛料中存在与蒂巴因分子量相近的化合物, 导致质谱在抓取母离子时无法准确分辨目标物, 出现相近干扰峰[18]; 或是样品中存在与蒂巴因化学结构相似的天然成分, 这些成分可能产生与蒂巴因相似的信号。由于这些信号与蒂巴因的信号在质谱图上难以区分, 因此可能导致假阳性结果的出现[19]。即使样品中实际上并不含有蒂巴因, 但由于这些相似成分的存在, 也可能被误判为含有蒂巴因。
2.3.2 飞行质谱筛查
使用了傅里叶变换质谱结合正压电喷雾电离对月桂叶与荜拨样品进行全质谱扫描, 扫描范围设置为100.0000~1200.0000 m/z。扫描结果如图2, 三者均有相近分子量的化合物, 因保留时间的不同, 可以初步判断三者为非手性的同分异构体, 可通过此推断可疑的化合物[20-23]。
2.3.3 干扰物质结构解析
在对干扰物进行结构解析时, 可使用其正负离子模式下的质荷比和加合离子信息在Chemspider官方网站(https://www.chemspider.com)上搜索可能的化合物[24-25]。蒂巴因的化学式为图3, 基于相近分子量, 容易在质谱端造成干扰[26], 易打碎为相同离子的分子量在311.375, 或同位素在314.393, 或分子量相同的同分异构体进行排查。共搜索到6种化合物, 如下表2所示, 疑似干扰物化学式为图4。对相应化合物进行购买验证。
通过以上可以看出, 月桂叶、荜拨的3种化学成分为同分异构体, 分子量与蒂巴因分子量极其相近。在一级质谱抓取目标物母离子时, 无法准确分辨, 会同时抓取相近分子量的化合物, 进入碰撞池进行打碎[27]。由于化学结构不同, 碰撞后打碎的子离子的数量有差异, 导致其最终丰度比与目标物范围不一致, 出现保留时间一致但丰度比不一致的假阳性问题[28]。
2.4 干扰物结果验证
在市场上仅购买到Launobine与Pisatin两种化合物, 经检测发现其未检测出蒂巴因假阳性情况, 见表3。干扰物可能存在于其他未购买到的化合物, 但由于市场管控, 无法进行购买, 仅排查该干扰物为香辛料中某种生物碱类化合物。
3 结论
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本研究对火锅底料中常用香辛料进行假阳性问题的排查, 发现月桂叶与荜拨中含有生物碱或酚类化合物, 其具有蒂巴因相似的化学结构以及分子量, 其在质谱图中呈现相似的峰形, 易于蒂巴因标准品产生交叉信号; 月桂叶提取物中存在保留时间(保留时间=4.454 min)与蒂巴因(保留时间=4.454 min)高度重叠(Δ保留时间<0.2 min)的干扰峰, 其分子量为311.381 ([M+H]⁺), 与蒂巴因理论值(311.375 Da)偏差仅<2 ppm; 荜拨中因含氨基侧链, 在质谱碎片离子上与蒂巴因部分匹配, 通过质谱分析原理, 易导致信号干扰[29-30]。
为进一步探究干扰机制, 本研究使用了傅里叶变换质谱结合正压电喷雾电离对月桂叶与荜拨样品进行了全质谱扫描, 推测三者为非手性的同分异构体。通过Chemspider官方网站搜索可能的化合物, 并对相应化合物进行购买验证, 但由于市场管制限制, 仅成功购买了Launobine与Pisatin两种化合物, 在本研究条件下并未发现它们能导致蒂巴因的假阳性情况。
综上所述, 本研究揭示了蒂巴因在质谱检测中可能受到香辛料中相似化学结构成分的干扰, 导致假阳性结果的出现。尽管对部分干扰物进行了排查, 但由于市场管控等原因, 未能完全确定干扰物的具体成分。因此, 在使用BJS 201802方法进行检测含有香辛料类样品时, 应考虑香辛料中生物碱类物质对蒂巴因干扰的情况。避免出现假阳性造成误判。未来将通过优化质谱条件、引入核磁共振技术及完善前处理流程, 提升检测特异性与准确性, 避免假阳性误判。
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2025年第16卷第13期
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20250119001
  • 接收时间：2025-01-19
  • 首发时间：2026-01-12
  • 出版时间：2025-07-15
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  • 收稿日期：2025-01-19
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    1 四川敏恩检测技术有限公司, 成都 611130
    2 成都圣恩生物科技股份有限公司, 成都 611130

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*蒋思雨(1997—), 女, 硕士, 助理工程师, 主要研究方向为食品安全检测。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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