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Article(id=1153986778802410292, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153986777279877909, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20241023003, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1729612800000, receivedDateStr=2024-10-23, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1753061488104, onlineDateStr=2025-07-21, pubDate=1736870400000, pubDateStr=2025-01-15, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1753061488104, onlineIssueDateStr=2025-07-21, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1753061488103, creator=13701087609, updateTime=1753061488103, updator=13701087609, issue=Issue{id=1153986777279877909, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='1', 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=1753061487741, creator=13701087609, updateTime=1757901302572, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1174286432060453412, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153986777279877909, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1174286432060453413, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153986777279877909, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=36, endPage=43, ext={EN=ArticleExt(id=1153986779196674876, articleId=1153986778802410292, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Determination of 15 kinds of chemicals illegally added in prefabricated food by ultra performance liquid chromatography-triple quadrupole composite linear ion trap mass spectrometry, columnId=1153986581653349021, journalTitle=Journal of Food Safety & Quality, columnName=Special Topic: Application of Modern Analysis Instrument in Food Detection, runingTitle=null, highlight=null, articleAbstract=

Objective To establish a method for the determination of 15 kinds of chemicals illegally added in prefabricated food by ultra performance liquid chromatography-triple quadrupole composite linear ion trap mass spectrometry in multiple reaction monitoring-information dependent acquisition-enhanced product ion (MRM-IDA-EPI) mode combined with pass-through solid phase extraction technology. Methods The samples were extracted with 1% (volume fraction) formic acid in acetonitrile. The extractive solution was purified by pass-through solid phase extraction column Captiva EMR-Lipid, and the purified liquid was separated on a Agilent Poroshell 120 EC-C18 (2.1 mm×100 mm, 1.9 μm) column. The mobile phase was acetonitrile and 5 mmol/L aqueous ammonium acetate containing 0.05% formic acid. The target compounds were detected by MRM-IDA-EPI mode with external standard method. Results The calibration curves of the 15 kinds of compounds were linear in the concentration range within limits with correlation coefficients between 0.9956 and 0.9996. The limits of detection ranged from 0.62-62.50 μg/kg. The average recoveries of 15 kinds of compounds at 3 different levels ranged from 78.33%-109.51% with accuracy of 0.67%-14.02%. Conclusion The method can be applied to the determination of 15 kinds of chemicals illegally added in prefabricated food with its rapidity, high accuracy and high precision, providing support for quality control and market regulation of prefabricated food.

, correspAuthors=Zhi-Mei LI, 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=Fang-Fang CHEN, Meng LIU, Liang ZHANG, Jing ZHANG, Mao-Yue KANG, Zhi-Mei LI), CN=ArticleExt(id=1153986797144101196, articleId=1153986778802410292, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=超高效液相色谱三重四极杆复合线性离子阱质谱法测定预制菜中15种非法添加化学药物, columnId=1153986778571723567, journalTitle=食品安全质量检测学报, columnName=专题：现代分析仪器在食品检测中的应用, runingTitle=null, highlight=null, articleAbstract=

目的 建立超高效液相色谱三重四极杆复合线性离子阱质谱法的多反应监测-信息依赖性采集-增强子离子扫描(multiple reaction monitoring-information dependent acquisition-enhanced product ion, MRM-IDA-EPI)方式结合通过型固相萃取技术测定预制菜中15种非法添加化学药物的方法。方法 样品用1%(体积分数)甲酸乙腈提取, 通过型固相萃取柱Captiva EMR-Lipid净化, 以乙腈-0.05%(体积分数)甲酸水(含5 mmol/L乙酸铵)为流动相, Agilent Poroshell 120 EC-C18 (2.1 mm×100 mm, 1.9 μm)色谱柱进行分离, 采用MRM-IDA-EPI的扫描方式, 外标法定量。结果 15种目标物在一定范围内, 线性相关系数范围为0.9956~0.9996。该方法的检出限在0.62~62.50 μg/kg。预制菜进行3个水平添加实验(n=6), 15种目标物的平均回收率为78.33%~109.51%, 精密度为0.67%~14.02%。结论 该方法简单快速, 准确度好, 精密度高, 适用于预制菜中非法添加15种化学药物的检测, 可为预制菜的质量检测及市场监管提供技术支撑。

, correspAuthors=李志梅, authorNote=null, correspAuthorsNote=
*李志梅(1975—), 女, 副主任药师, 主要研究方向为食品、药品仪器分析检测。E-mail:
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陈芳芳(1989—), 女, 硕士, 主管药师, 主要研究方向为食品、药品仪器分析检测。E-mail:

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陈芳芳(1989—), 女, 硕士, 主管药师, 主要研究方向为食品、药品仪器分析检测。E-mail:

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陈芳芳(1989—), 女, 硕士, 主管药师, 主要研究方向为食品、药品仪器分析检测。E-mail:

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Journal of Food Safety & Quality, 2018, 9(1): 107-115., articleTitle=Simultaneous determination of 5 kinds of pericarpium papaveris alkaloids and 6 kinds of industrial dyes in snack foods and hot pot seasoning by ultra performance liquid chromatography- tandem mass spectromentry, refAbstract=null), Reference(id=1174369575476019750, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, doi=null, pmid=null, pmcid=null, year=2024, volume=22, issue=9, pageStart=2438, pageEnd=2446, url=null, language=null, rfNumber=[30], rfOrder=54, authorNames=姚奕然, 蒋凡, 刘欢欢, journalName=中南药学, refType=null, unstructuredReference=姚奕然, 蒋凡, 刘欢欢, 等. 基于UPLC-MRM-IDA-EPI法高通量筛查保健食品中60种非法添加的化学药物[J]. 中南药学, 2024, 22(9): 2438-2446., articleTitle=基于UPLC-MRM-IDA-EPI法高通量筛查保健食品中60种非法添加的化学药物, refAbstract=null), Reference(id=1174369575547322919, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, doi=null, pmid=null, pmcid=null, year=2024, volume=22, issue=9, pageStart=2438, pageEnd=2446, url=null, language=null, rfNumber=[30], rfOrder=55, authorNames=YAO YR, JIANG F, LIU HH, journalName=Central South Pharmacy, refType=null, unstructuredReference=YAO YR, JIANG F, LIU HH, et al. High-throughput screening and rapid quantification of 60 illegally added chemical drugs in dietary supplements by UPLC-MRM-IDA-EPI[J]. Central South Pharmacy, 2024, 22(9): 2438-2446., articleTitle=High-throughput screening and rapid quantification of 60 illegally added chemical drugs in dietary supplements by UPLC-MRM-IDA-EPI, refAbstract=null)], funds=[Fund(id=1174369571168469486, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, awardId=CY2022227, language=CN, fundingSource=浙江省市场监督管理局雏鹰计划核心项目(CY2022227), fundOrder=null, country=null), Fund(id=1174369571239772655, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, awardId=2024006, language=CN, fundingSource=温州市市场监督管理局科技计划项目(2024006), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1174369567691391414, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, xref=null, ext=[AuthorCompanyExt(id=1174369567695585719, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, companyId=1174369567691391414, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Wenzhou Institute for Food and Drug Control, Wenzhou 325000, China), AuthorCompanyExt(id=1174369567699780024, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, companyId=1174369567691391414, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=温州市食品药品检验科学研究院, 温州 325000)])], figs=[ArticleFig(id=1174369569843069410, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, language=EN, label=Fig.1, caption=Chromatogram of the 15 kinds of compounds, figureFileSmall=F3N1wnlIWDKYPUQ78MmCyQ==, figureFileBig=JH9BvtRTxYIvx4iDRosJNQ==, tableContent=null), ArticleFig(id=1174369569973092835, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, language=CN, label=图1, caption=15种目标化合物色谱图

注: 1~15分别代表吗啡、对乙酰氨基酚、氨基比林、可待因、咖啡因、安替比林、阿司匹林 、蒂巴因、罂粟碱、非那西丁、苯巴比妥、那可丁、氯苯那敏、异丙安替比林、双氯芬酸钠。

, figureFileSmall=F3N1wnlIWDKYPUQ78MmCyQ==, figureFileBig=JH9BvtRTxYIvx4iDRosJNQ==, tableContent=null), ArticleFig(id=1174369570061173220, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, language=EN, label=Fig.2, caption=Matrix effects of the compounds, figureFileSmall=gw4EadkmfPtumbgYjEkiXg==, figureFileBig=/6aCRd9OcBIv4boPQtwxcg==, tableContent=null), ArticleFig(id=1174369570145059301, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, language=CN, label=图2, caption=各目标化合物的基质效应, figureFileSmall=gw4EadkmfPtumbgYjEkiXg==, figureFileBig=/6aCRd9OcBIv4boPQtwxcg==, tableContent=null), ArticleFig(id=1174369570216362470, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, language=EN, label=Fig.3, caption=Secondary mass spectrogram of positive samples and reference standards, figureFileSmall=naiDs3uCfAcJcqx/OGeppA==, figureFileBig=qSpGttbh7zhDRXx3Y9XSDg==, tableContent=null), ArticleFig(id=1174369570283471335, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, language=CN, label=图3, caption=阳性样品与标准品的二级质谱图, figureFileSmall=naiDs3uCfAcJcqx/OGeppA==, figureFileBig=qSpGttbh7zhDRXx3Y9XSDg==, tableContent=null), ArticleFig(id=1174369570379940328, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, language=EN, label=Table 1, caption=

Mass spectrometric parameters for the 15 kinds of analytes

, figureFileSmall=null, figureFileBig=null, tableContent=
序号 保留时间/min 化合物名称 扫描方式 母离子(m/z) 子离子(m/z) 去簇电压/V 碰撞能量/eV
1 1.02 吗啡 ESI+ 286.0 181.1*/165.1 97 47/51
2 1.52 对乙酰氨基酚 ESI+ 152.1 110.0*/93.0 160 23/31
3 2.09 氨基比林 ESI+ 232.0 96.9*/113.0 160 43/19
4 2.22 可待因 ESI+ 300.0 215.1*/165.2 90 34/55
5 2.83 咖啡因 ESI+ 195.1 138.1*/110.0 70 27/32
6 5.05 安替比林 ESI+ 189.0 56.0*/77.0 60 27/37
7 6.06 阿司匹林 ESI- 179.0 93.0*/137.0 -60 -25/-11
8 6.05 蒂巴因 ESI+ 312.0 58.2*/251.0 52 48/40
9 6.84 罂粟碱 ESI+ 340.2 202.1*/171.1 92 36/40
10 6.86 非那西丁 ESI+ 180.1 138.0*/110.0 160 21/22
11 6.99 苯巴比妥 ESI- 231.1 42.0*/188.0 -50 -40/-15
12 7.04 那可丁 ESI+ 414.2 220.2*/353.1 95 30/34
13 7.10 氯苯那敏 ESI+ 275.2 230.1*/167.1 50 22/53
14 8.82 异丙安替比林 ESI+ 231.0 189.0*/146.0 70 28/34
15 11.04 双氯芬酸钠 ESI+ 296.1 250.0*/215.0 80 18/25
), ArticleFig(id=1174369570459632105, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, language=CN, label=表1, caption=

15种目标物的质谱检测参数

, figureFileSmall=null, figureFileBig=null, tableContent=
序号 保留时间/min 化合物名称 扫描方式 母离子(m/z) 子离子(m/z) 去簇电压/V 碰撞能量/eV
1 1.02 吗啡 ESI+ 286.0 181.1*/165.1 97 47/51
2 1.52 对乙酰氨基酚 ESI+ 152.1 110.0*/93.0 160 23/31
3 2.09 氨基比林 ESI+ 232.0 96.9*/113.0 160 43/19
4 2.22 可待因 ESI+ 300.0 215.1*/165.2 90 34/55
5 2.83 咖啡因 ESI+ 195.1 138.1*/110.0 70 27/32
6 5.05 安替比林 ESI+ 189.0 56.0*/77.0 60 27/37
7 6.06 阿司匹林 ESI- 179.0 93.0*/137.0 -60 -25/-11
8 6.05 蒂巴因 ESI+ 312.0 58.2*/251.0 52 48/40
9 6.84 罂粟碱 ESI+ 340.2 202.1*/171.1 92 36/40
10 6.86 非那西丁 ESI+ 180.1 138.0*/110.0 160 21/22
11 6.99 苯巴比妥 ESI- 231.1 42.0*/188.0 -50 -40/-15
12 7.04 那可丁 ESI+ 414.2 220.2*/353.1 95 30/34
13 7.10 氯苯那敏 ESI+ 275.2 230.1*/167.1 50 22/53
14 8.82 异丙安替比林 ESI+ 231.0 189.0*/146.0 70 28/34
15 11.04 双氯芬酸钠 ESI+ 296.1 250.0*/215.0 80 18/25
), ArticleFig(id=1174369570535129578, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, language=EN, label=Table 2, caption=

Linear ranges, correlation coefficients, linear equations and limits of detection

, figureFileSmall=null, figureFileBig=null, tableContent=
被测化合物 线性范围/(ng/mL) 回归方程 相关系数(r) 检出限/(μg/kg)
对乙酰氨基酚 5.0~125.0 Y=1.317×104X+5.535×103 0.9995 1.25
氯苯那敏 5.0~125.0 Y=5.523×104X+6.374×103 0.9995 3.12
双氯芬酸钠 5.0~125.0 Y=3.045×103X+5.692×102 0.9993 6.25
氨基比林 5.0~200.0 Y=8.366×103X-7.476×101 0.9987 3.12
安替比林 5.0~250.0 Y=4.047×103X+4.012×101 0.9989 3.12
非那西丁 5.0~125.0 Y=2.903×104X+9.644×103 0.9988 1.25
咖啡因 5.0~125.0 Y=1.155×104X+5.247×102 0.9995 3.12
异丙安替比林 5.0~125.0 Y=3.811×104X+7.905×103 0.9985 1.25
罂粟碱 1.0~40.0 Y=5.969×104X-9.580×101 0.9996 0.62
吗啡 5.0~125.0 Y=2.356×103X+3.247×102 0.9988 3.12
那可丁 1.0~40.0 Y=7.349×104X+7.312×101 0.9990 0.62
可待因 5.0~200.0 Y=5.420×103X+1.776×103 0.9986 3.12
蒂巴因 1.0~40.0 Y=2.443×104X+3.668×103 0.9956 0.62
苯巴比妥 5.0~250.0 Y=9.296×102X+8.637×101 0.9993 6.25
阿司匹林 50.0~2500.0 Y=9.075×101X+3.630×101 0.9977 62.50
), ArticleFig(id=1174369570644181483, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, language=CN, label=表2, caption=

线性范围、相关系数、回归方程和检出限

, figureFileSmall=null, figureFileBig=null, tableContent=
被测化合物 线性范围/(ng/mL) 回归方程 相关系数(r) 检出限/(μg/kg)
对乙酰氨基酚 5.0~125.0 Y=1.317×104X+5.535×103 0.9995 1.25
氯苯那敏 5.0~125.0 Y=5.523×104X+6.374×103 0.9995 3.12
双氯芬酸钠 5.0~125.0 Y=3.045×103X+5.692×102 0.9993 6.25
氨基比林 5.0~200.0 Y=8.366×103X-7.476×101 0.9987 3.12
安替比林 5.0~250.0 Y=4.047×103X+4.012×101 0.9989 3.12
非那西丁 5.0~125.0 Y=2.903×104X+9.644×103 0.9988 1.25
咖啡因 5.0~125.0 Y=1.155×104X+5.247×102 0.9995 3.12
异丙安替比林 5.0~125.0 Y=3.811×104X+7.905×103 0.9985 1.25
罂粟碱 1.0~40.0 Y=5.969×104X-9.580×101 0.9996 0.62
吗啡 5.0~125.0 Y=2.356×103X+3.247×102 0.9988 3.12
那可丁 1.0~40.0 Y=7.349×104X+7.312×101 0.9990 0.62
可待因 5.0~200.0 Y=5.420×103X+1.776×103 0.9986 3.12
蒂巴因 1.0~40.0 Y=2.443×104X+3.668×103 0.9956 0.62
苯巴比妥 5.0~250.0 Y=9.296×102X+8.637×101 0.9993 6.25
阿司匹林 50.0~2500.0 Y=9.075×101X+3.630×101 0.9977 62.50
), ArticleFig(id=1174369570790982124, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, language=EN, label=Table 3, caption=

Average recoveries and precisions of the components (n=6)

, figureFileSmall=null, figureFileBig=null, tableContent=
被测物 低浓度 中浓度 高浓度
加标量/
(μg/kg)		 回收率
/%		 RSDs
/%		 加标量
/(μg/kg)		 回收率
/%		 RSDs
/%		 加标量
/(μg/kg)		 回收率
/%		 RSDs
/%
对乙酰氨基酚 12.5 97.10 10.34 125 92.93 5.23 312.5 87.96 6.32
氯苯那敏 12.5 84.52 8.06 125 79.35 5.77 312.5 87.46 7.01
双氯芬酸钠 62.5 78.33 5.12 250 80.82 4.45 500.0 79.53 1.83
氨基比林 12.5 94.96 4.85 125 86.54 2.08 312.5 92.47 3.46
安替比林 12.5 85.42 5.42 125 83.86 5.42 312.5 88.18 8.42
非那西丁 12.5 109.51 4.10 125 102.15 6.27 312.5 92.59 1.09
咖啡因 12.5 96.47 9.63 125 92.94 4.91 312.5 101.42 3.52
异丙安替比林 12.5 88.80 14.02 125 98.87 6.10 312.5 95.61 8.17
罂粟碱 2.5 91.16 6.47 25 92.19 8.86 62.5 89.83 5.73
吗啡 12.5 95.31 9.32 125 85.53 8.23 312.5 80.74 3.60
那可丁 2.5 90.63 7.52 25 89.62 7.90 62.5 89.87 8.11
可待因 12.5 103.54 7.26 125 88.72 6.52 312.5 92.68 4.09
蒂巴因 2.5 92.39 9.50 25 89.30 1.91 62.5 80.10 1.62
苯巴比妥 62.5 87.41 10.03 250 95.62 3.07 500.0 93.72 0.67
阿司匹林 625.0 104.74 7.71 2500 96.91 4.18 5000.0 104.80 4.75
), ArticleFig(id=1174369570971337197, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986778802410292, language=CN, label=表3, caption=

方法的回收率及精密度(n=6)

, figureFileSmall=null, figureFileBig=null, tableContent=
被测物 低浓度 中浓度 高浓度
加标量/
(μg/kg)		 回收率
/%		 RSDs
/%		 加标量
/(μg/kg)		 回收率
/%		 RSDs
/%		 加标量
/(μg/kg)		 回收率
/%		 RSDs
/%
对乙酰氨基酚 12.5 97.10 10.34 125 92.93 5.23 312.5 87.96 6.32
氯苯那敏 12.5 84.52 8.06 125 79.35 5.77 312.5 87.46 7.01
双氯芬酸钠 62.5 78.33 5.12 250 80.82 4.45 500.0 79.53 1.83
氨基比林 12.5 94.96 4.85 125 86.54 2.08 312.5 92.47 3.46
安替比林 12.5 85.42 5.42 125 83.86 5.42 312.5 88.18 8.42
非那西丁 12.5 109.51 4.10 125 102.15 6.27 312.5 92.59 1.09
咖啡因 12.5 96.47 9.63 125 92.94 4.91 312.5 101.42 3.52
异丙安替比林 12.5 88.80 14.02 125 98.87 6.10 312.5 95.61 8.17
罂粟碱 2.5 91.16 6.47 25 92.19 8.86 62.5 89.83 5.73
吗啡 12.5 95.31 9.32 125 85.53 8.23 312.5 80.74 3.60
那可丁 2.5 90.63 7.52 25 89.62 7.90 62.5 89.87 8.11
可待因 12.5 103.54 7.26 125 88.72 6.52 312.5 92.68 4.09
蒂巴因 2.5 92.39 9.50 25 89.30 1.91 62.5 80.10 1.62
苯巴比妥 62.5 87.41 10.03 250 95.62 3.07 500.0 93.72 0.67
阿司匹林 625.0 104.74 7.71 2500 96.91 4.18 5000.0 104.80 4.75
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超高效液相色谱三重四极杆复合线性离子阱质谱法测定预制菜中15种非法添加化学药物
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陈芳芳 , 刘萌 , 张亮 , 张晶 , 康茂约 , 李志梅 *
食品安全质量检测学报 | 专题：现代分析仪器在食品检测中的应用 2025,16(1): 36-43
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食品安全质量检测学报 | 专题：现代分析仪器在食品检测中的应用 2025, 16(1): 36-43
超高效液相色谱三重四极杆复合线性离子阱质谱法测定预制菜中15种非法添加化学药物
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陈芳芳 , 刘萌, 张亮, 张晶, 康茂约, 李志梅*
作者信息
  • 温州市食品药品检验科学研究院, 温州 325000

    • 陈芳芳(1989—), 女, 硕士, 主管药师, 主要研究方向为食品、药品仪器分析检测。E-mail:

通讯作者:

*李志梅(1975—), 女, 副主任药师, 主要研究方向为食品、药品仪器分析检测。E-mail:
Determination of 15 kinds of chemicals illegally added in prefabricated food by ultra performance liquid chromatography-triple quadrupole composite linear ion trap mass spectrometry
Fang-Fang CHEN , Meng LIU, Liang ZHANG, Jing ZHANG, Mao-Yue KANG, Zhi-Mei LI*
Affiliations
  • Wenzhou Institute for Food and Drug Control, Wenzhou 325000, China
出版时间: 2025-01-15 doi: 10.19812/j.cnki.jfsq11-5956/ts.20241023003
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摘要
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目的 建立超高效液相色谱三重四极杆复合线性离子阱质谱法的多反应监测-信息依赖性采集-增强子离子扫描(multiple reaction monitoring-information dependent acquisition-enhanced product ion, MRM-IDA-EPI)方式结合通过型固相萃取技术测定预制菜中15种非法添加化学药物的方法。方法 样品用1%(体积分数)甲酸乙腈提取, 通过型固相萃取柱Captiva EMR-Lipid净化, 以乙腈-0.05%(体积分数)甲酸水(含5 mmol/L乙酸铵)为流动相, Agilent Poroshell 120 EC-C18 (2.1 mm×100 mm, 1.9 μm)色谱柱进行分离, 采用MRM-IDA-EPI的扫描方式, 外标法定量。结果 15种目标物在一定范围内, 线性相关系数范围为0.9956~0.9996。该方法的检出限在0.62~62.50 μg/kg。预制菜进行3个水平添加实验(n=6), 15种目标物的平均回收率为78.33%~109.51%, 精密度为0.67%~14.02%。结论 该方法简单快速, 准确度好, 精密度高, 适用于预制菜中非法添加15种化学药物的检测, 可为预制菜的质量检测及市场监管提供技术支撑。

非法添加物  /  预制菜  /  通过型固相萃取  /  线性离子阱质谱法  /  多反应监测-信息依赖性采集-增强子离子扫描

Objective To establish a method for the determination of 15 kinds of chemicals illegally added in prefabricated food by ultra performance liquid chromatography-triple quadrupole composite linear ion trap mass spectrometry in multiple reaction monitoring-information dependent acquisition-enhanced product ion (MRM-IDA-EPI) mode combined with pass-through solid phase extraction technology. Methods The samples were extracted with 1% (volume fraction) formic acid in acetonitrile. The extractive solution was purified by pass-through solid phase extraction column Captiva EMR-Lipid, and the purified liquid was separated on a Agilent Poroshell 120 EC-C18 (2.1 mm×100 mm, 1.9 μm) column. The mobile phase was acetonitrile and 5 mmol/L aqueous ammonium acetate containing 0.05% formic acid. The target compounds were detected by MRM-IDA-EPI mode with external standard method. Results The calibration curves of the 15 kinds of compounds were linear in the concentration range within limits with correlation coefficients between 0.9956 and 0.9996. The limits of detection ranged from 0.62-62.50 μg/kg. The average recoveries of 15 kinds of compounds at 3 different levels ranged from 78.33%-109.51% with accuracy of 0.67%-14.02%. Conclusion The method can be applied to the determination of 15 kinds of chemicals illegally added in prefabricated food with its rapidity, high accuracy and high precision, providing support for quality control and market regulation of prefabricated food.

illegal additives  /  prefabricated food  /  pass-through solid phase extraction  /  linear ion trap mass spectrometry  /  multiple reaction monitoring-information dependent acquisition-enhanced product ion
陈芳芳, 刘萌, 张亮, 张晶, 康茂约, 李志梅. 超高效液相色谱三重四极杆复合线性离子阱质谱法测定预制菜中15种非法添加化学药物. 食品安全质量检测学报, 2025 , 16 (1) : 36 -43 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241023003
Fang-Fang CHEN, Meng LIU, Liang ZHANG, Jing ZHANG, Mao-Yue KANG, Zhi-Mei LI. Determination of 15 kinds of chemicals illegally added in prefabricated food by ultra performance liquid chromatography-triple quadrupole composite linear ion trap mass spectrometry[J]. Journal of Food Safety & Quality, 2025 , 16 (1) : 36 -43 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241023003
正文
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0 引言
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随着生活节奏加快, 近年来预制菜行业发展迅猛。2023年中国预制菜市场规模为5165亿元, 同比增长23.1%, 预计2026年市场规模超万亿元[1]。近年来, 新闻中不时报道火锅底料、卤菜、卤水汤料、酱料等食品及食品调料中添加罂粟壳、头痛粉等非法成分。预制菜作为新兴产业, 行业准入门槛低, 加工工艺良莠不齐, 部分商家缺乏法律意识, 一味追求利润, 不追求质量, 故而预制菜也有可能是商家非法添加的目标对象。食品非法添加物是指未经相关法律法规允许, 或超出规定使用范围和限量, 被人为添加到食品中的化学合成物或天然提取物[2]。食品中常见的非法添加物有罂粟壳、头痛粉和一些非食品级的工业原料如苏丹红、三聚氰胺[3]。罂粟壳是罂粟科植物罂粟经干燥处理后的成熟果壳, 含有吗啡、罂粟碱、可待因、蒂巴因、那可丁等生物碱类物质。长期食用含有此类物质的食品不仅会使人成瘾, 还会导致慢性中毒, 损害人体某些器官系统的正常功能[4-5]。头痛粉又称阿咖酚散, 是一种具有解热镇痛作用的非处方药品, 含有对乙酰氨基酚、阿司匹林、咖啡因等化学成分。长期摄入含有此类药物的食品除了会产生一些不良反应, 更甚者引起急性毒性, 对肝脏、肾脏等器官造成不可逆的损害[6-7], 严重危害消费者的身体健康。因此, 加强对预制菜中非法添加化学药物的监管非常重要。
目前, 检测非法添加化学药物的相关文献报道主要采用高效液相色谱-串联质谱法[3,5,8-9]、液相色谱法[4,10-11]、气相色谱法[12-13]、气相色谱-串联质谱法[14-15], 其中高效液相色谱-串联质谱法是近年来的研究热点。传统超高效液相色谱三重四极杆质谱法采用多反应监测(multiple reaction monitoring, MRM)模式进行化合物的定性和定量测定, 具有分离效果好, 灵敏度高等优点, 因而广泛用于农兽药残留以及非法添加等的检测。但预制菜食品基质复杂, 可能会出现假阳性和假阴性等情况。超高效液相色谱三重四极杆复合线性离子阱质谱法采用多反应监测触发增强子离子扫描(multiple reaction monitoring- information dependent acquisition-enhanced product ion, MRM-IDA-EPI)方式, 与传统方法相比, 可以在准确定量的同时, 采集目标化合物的高质量二级质谱图, 与谱库比对, 获得更精准的定性确证, 大大提高了检测准确率和效率[16-17]。
本研究采用超高效液相色谱三重四极杆复合线性离子阱质谱法的MRM-IDA-EPI扫描方式, 结合通过型固相萃取技术, 建立了同时测定预制菜中15种非法添加化学药物的检测方法, 为预制菜食品安全监管相关政策的制定和相关检测标准的建立提供数据支撑和理论依据。
1 材料与方法
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1.1 仪器与试剂
QTRAP-5500三重四极杆/复合线性离子阱质谱仪[配有电喷雾离子源(electrospray ionization, ESI)及Multiquant 3.0.3数据处理系统](美国AB SCIEX公司); BSA822电子天平(感量0.01 g, 德国赛多利斯公司); XSR205DU电子天平[感量0.01 mg, 梅特勒-托利多仪器(上海)有限公司]; Multi Reax EU振荡器(德国Heidolph仪器设备有限公司); CF16RN离心机(日本HITACHI公司); KQ-600DE超声波清洗器(昆山市超声仪器有限公司); AutoEVA-60全自动平行浓缩仪[睿科集团(厦门)股份有限公司]; Milli-Q IQ 7000超纯水仪(美国Millipore公司); Captiva EMR-Lipid 6 mL/600 mg固相萃取柱、EMR-Polish管、PTFE-Q亲水性滤膜(0.22 μm)、Agilent Poroshell 120 EC-C18色谱柱(2.1 mm× 100 mm, 1.9 μm)(美国Agilent公司)。
标准品: 吗啡(1.0 mg/mL)、蒂巴因(1.0 mg/mL)(美国Cerilliant公司); 可待因(100 μg/mL)、非那西丁(纯度98.1%)(美国Stanford Chemicals公司); 盐酸罂粟碱(100 μg/mL)、那可丁盐酸盐水合物(纯度99.90%)(中国坛墨质检科技股份有限公司); 咖啡因(含量99.7%)、对乙酰氨基酚(含量99.9%)、氨基比林(含量99.7%)、安替比林(含量99.9%)、阿司匹林(含量99.8%)、苯巴比妥(含量99.7%)、马来酸氯苯那敏(含量99.7%)、异丙安替比林(含量100%)、双氯芬酸钠(含量100.0%)(中国食品药品检定研究院)。
乙腈(色谱纯, 美国Spectrum公司); 甲酸(质谱纯, 上海阿拉丁生化科技股份有限公司); 乙酸铵(高纯度生化试剂, 美国Sigma-Aldrich公司)。
1.2 样品
预制菜样品均购自温州市本地企业, 共45批, 其中速冻生制调制肉制品15批, 腌腊肉制品15批, 炖卤肉制品15批。
1.3 实验方法
1.3.1 标准溶液配制
(1)标准储备溶液
分别准确称取氨基比林、咖啡因、安替比林、阿司匹林、对乙酰氨基酚、非那西丁、苯巴比妥、马来酸氯苯那敏(折算为氯苯那敏)、异丙安替比林、那可丁盐酸盐水合物(折算为那可丁)与双氯芬酸钠11种标准物质适量, 用甲醇溶解并定容至10 mL容量瓶, 得到质量浓度约为1000 μg/mL的标准储备液, -18 ℃避光储存。
(2)混合标准工作溶液
分别吸取储备液适量用空白样品提取液或10%(体积分数)乙腈水溶液逐级稀释至罂粟碱、那可丁、蒂巴因质量浓度为1.0、5.0、10.0、20.0、25.0、40.0、50.0 ng/mL, 阿司匹林质量浓度为50.0、250.0、500.0、1000.0、1250.0、2000.0、2500.0 ng/mL, 其余化合物质量浓度为5.0、25.0、50.0、100.0、125.0、200.0、250.0 ng/mL的混合标准工作溶液。
1.3.2 样品制备
准确称取泥状试样2 g(精确至0.01 g)于50 mL离心管中, 加水3 mL和陶瓷均质子, 振摇1 min使分散均匀, 加10 mL 1%甲酸乙腈振荡1 min后, 超声10 min。加入盐析包(4 g无水硫酸镁、1 g氯化钠、1 g柠檬酸钠、0.5 g柠檬酸二钠盐)盐析分层, 以8000 r/min速率4 ℃离心5 min。准确吸取4 mL乙腈层上清液, 准确加入水1 mL, 摇匀, 加入到Captiva EMR-Lipid固相萃取柱中, 收集全部流出液到EMR-Polish管(氯化钠、硫酸镁)中, 快速剧烈振荡, 涡旋1 min, 5000 r/min低温离心10 min, 吸取2.00 mL上清液于离心管中, 氮吹至近干(45 ℃), 用1.00 mL 10%乙腈水溶液溶解残渣, 涡旋混匀, 经PTFE-Q亲水性滤膜(0.22 μm)过滤, 上机测定。
1.3.3 分析条件
(1)色谱条件
色谱柱: Agilent Poroshell 120 EC-C18 (2.1 mm× 100 mm, 1.9 μm)。流动相A: 0.05%(体积分数)甲酸水(含5 mmol/L乙酸铵); 流动相B: 乙腈; 流速: 0.3 mL/min; 进样量: 1 μL; 柱温: 35 ℃。梯度洗脱程序0~2.0 min, 10% B; 2.0~6.0 min, 10%~30% B; 6.0~9.0 min, 30%~50% B; 9.0~11.5 min, 50%~95% B; 11.5~14.5 min, 95% B; 14.5~15.0 min, 95%~10% B; 15.0~20.0 min, 10% B。
(2)质谱条件
离子源: ESI; 扫描方式: 正离子和负离子同时扫描; 检测方式: MRM-IDA-EPI的模式; 离子源温度: 400 ℃; 气帘气: 35 Psi; 碰撞气: 高; 喷雾电压: 5500 V (ESI+), 4500 V (ESI-); 雾化气: 50 Psi; 辅助气: 55 Psi。以MRM-IDA-EPI模式进行扫描, 具体质谱参数见表1。IDA执行动态背景扣除; 扫描阈值100 cps; EPI源参数与MRM模式一致; 去簇电压为80 V; 碰撞能量为(35±15) eV; 扫描范围50~500 u。
1.4 数据处理
采用Analyst 1.7软件对样品进行采集分析, Multiquant 3.0.3软件对采集和检测结果进行数据处理分析。
2 结果与分析
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2.1 前处理条件优化
2.1.1 提取溶剂的选择
预制菜成分复杂, 含有很多调味料和油脂, 提取前先加水将样品打散, 使后续加入的提取溶剂能够与样品充分接触以提高提取效率[18-19]。一般用甲醇、乙腈和乙酸乙酯等作为提取溶剂。甲醇与水互溶, 不能分层, 乙酸乙酯提取的油脂等杂质较多, 而乙腈相较于其他提取溶剂有以下优点: 乙腈对大多数被测物提取效果较好, 能使蛋白质变性沉降, 具有较好的去除蛋白效果, 且盐析能实现乙腈与水相分离, 无需溶剂转换。与纯乙腈相比, 提取溶剂中加入适量的酸, 使提取介质呈酸性, 既能够防止部分被测物在碱性条件下降解, 又能与待测物的碱基反应成盐, 还能去除部分杂质, 从而改善提取效果[20-21]。本研究比较了乙腈、0.1%甲酸乙腈、0.5%甲酸乙腈、1%甲酸乙腈和2%甲酸乙腈5种溶剂的提取效果。结果表明, 大部分目标物的回收率随着甲酸质量分数的增加而逐渐提高, 但苯巴比妥和阿司匹林为负离子扫描模式, 甲酸会对其产生抑制作用, 苯巴比妥、阿司匹林的响应随着甲酸质量分数的进一步增加反而显著降低。用1%甲酸乙腈作为提取溶剂时, 目标化合物的回收率整体较好。因此, 综合考虑, 本研究采用1%甲酸乙腈体系进行提取。
2.1.2 净化方式的选择
目前化学药物检测分析的净化方法主要有液液萃取法、固相萃取法、QuEChERS和Captiva EMR-Lipid等[21-22]。与传统的固相萃取柱相比, Captiva EMR-Lipid固相萃取柱有机试剂消耗少, 直接上样、重力自流、收集全部流出液, 无需活化、淋洗、洗脱, 操作简单, 省时省力, 大大简化了前处理步骤, 实验效率显著提高[23-24]。预制菜中蛋白质含量较高, 对检测结果有较大干扰, 本研究在提取过程中加入盐析包(4 g无水硫酸镁、1 g氯化钠、1 g柠檬酸钠、0.5 g柠檬酸二钠盐), 降低蛋白质的溶解度, 使蛋白质凝聚析出而沉淀, 降低蛋白质对样品检测结果的干扰。预制菜中还有大量的脂肪、色素等干扰物质。Captiva EMR-Lipid净化柱是一种新型的增强型脂质去除净化柱, 可高选择性、高效率地捕获脂质, 减少对待测物的吸附, 同时可去除部分色素。过柱后再加入到EMR-Polish管中, 离心、氮吹等操作能进一步净化样品, 排除脂肪、蛋白质、色素等物质的干扰。因此, 本研究的净化方式选用Captiva EMR-Lipid萃取柱。
2.1.3 复溶溶剂的选择
本研究比较了乙腈、90%乙腈水、10%乙腈水为复溶溶剂时, 待测化合物定量离子和定性离子的色谱峰响应和峰形。结果发现, 用乙腈或90%乙腈水复溶时有较强的溶剂效应, 色谱峰存在肩峰、峰拖尾、峰分叉等情况; 选用10%乙腈水复溶时, 峰形对称, 半峰宽窄, 分离度符合要求。因此, 本研究选用10%乙腈水作为复溶溶剂。
2.1.4 滤膜的选择
将25.0 ng/mL的罂粟碱、那可丁、蒂巴因, 1250.0 ng/mL阿司匹林, 其余化合物质量浓度为125.0 ng/mL的混合标准溶液分别经有机尼龙滤膜(0.22 μm)和Agilent PTFE-Q亲水性滤膜(0.22 μm)过滤后直接上机测定。结果表明, 有机尼龙滤膜对双氯芬酸钠有很强的吸附作用, 损失率达95%以上, 对苯巴比妥和阿司匹林也有一定的吸附作用; Agilent PTFE-Q亲水性滤膜过滤后15种目标物的回收率在80%~110%, 因此用Agilent PTFE-Q亲水性滤膜过滤。
2.2 色谱条件优化
2.2.1 色谱柱的选择
本研究考察了Agilent Poroshell 120 EC-C18 (2.1 mm× 100 mm, 1.9 μm)和Agilent SB-C18 RRHD (2.1 mm×100 mm, 1.8 μm)的分离效果, 发现在乙腈-甲酸乙酸铵水流动相体系内, 两根柱子的分离效果差不多, 但前者的半峰宽更小, 峰形更尖锐, 15种化合物的色谱图如图1所示。后者氯苯那敏峰形拖尾, 氨基比林峰形分叉, 苯巴比妥响应降低为柱1的60%~70%, 阿司匹林响应非常差, 仅为前者的1/10。故本研究选择Agilent Poroshell 120 EC-C18柱进行分离。
2.2.2 流动相的选择
本研究比较了乙腈-水、乙腈-甲酸水、乙腈-乙酸铵水、乙腈-甲酸乙酸铵水4种流动相体系。根据目标化合物的响应、峰形、分离度等综合评价, 采用甲酸乙酸铵水-乙腈作为流动相时, 15种化合物的响应信号较高, 峰形较好, 分离度亦能满足要求。为进一步确定最佳的流动相组成, 比较了同一浓度混合标准溶液在甲酸体积分数分别为0.01%、0.02%、0.05%、0.10%、0.20%、0.50%时各组分响应值的变化情况。结果表明, 正离子模式采集的化合物的响应随着甲酸体积分数的增加而增强, 但流动相中甲酸的加入会抑制苯巴双妥、阿司匹林等负离子模式采集的化合物的响应。乙酸铵具有较强的缓冲能力, 可使流动相保持一定的pH及离子强度, 减少拖尾, 改善峰形。综合考虑, 本研究采用乙腈-0.05%甲酸水溶液(含5 mmol/L乙酸铵)作为流动相。
2.3 基质效应
基质效应对液相色谱-质谱联用法结果准确度有重要影响[25]。基质效应是指由于分析物以外其他组分的存在或其他物理、化学因素直接或间接影响离子化效果, 从而使待测物响应增大或减小的现象[20]。为评估基质效应的大小, 分别用空白基质提取液和溶剂(10%乙腈水溶液)配制成各标准曲线点浓度相同的两条标准曲线, 以外标法做线性分析, 基质效应(%)用基质标准曲线斜率与溶剂标准曲线斜率的百分比进行评估[26]。当基质效应在85%~115%范围内, 可认为不存在基质效应或基质效应不明显[26-29]。由图2可见, 除了那可丁的基质效应为132%, 略大, 其余化合物的基质效应均在85%~115%范围内, 较好地消除了基质效应。考虑到不同基质的基质效应会有差异, 采用基质标准曲线也难以兼顾所有类型的基质, 那可丁的基质效应中等偏弱, 因此, 本研究采用溶剂标准曲线, 在简化实验步骤的同时, 使定性结果和定量结果更加准确可靠。
2.4 EPI数据定性分析
传统的MRM模式根据相对保留时间和相对离子丰度比(定性离子与定量离子的响应值之比)来进行定性分析。线性离子阱具有对目标离子捕获、富集等功能, 在定性分析方面比传统三重四极杆更有优势。以咖啡因为例, MRM模式下咖啡因在2.83 min出峰, [M+H]+获得质荷比为195.1的母离子, 碰撞解离后产生碎片离子, 以138.1为定量离子, 110.0为定性离子。在MRM-IDA-EPI模式下, 咖啡因中更多的碎片离子被准确识别, 如163.1、135.0、91.9、76.9等。碎片信息越丰富, 在进行化合物确证时, 准确度越高, 出现假阳性的概率越低[30]。采用MRM-IDA-EPI模式, 采集了15种目标化合物标准物质的二级质谱图, 添加到谱库中, 用于定性确证。当依据MRM的保留时间和离子丰度比判断为疑似阳性样品时, 进一步结合疑似阳性样品的二级质谱图与谱库标准谱图进行比对(如图3为阳性样品与标准品的二级质谱图), 比较二者的特征离子及其强度, 避免假阳性的误判。
为减少假阳性情况的出现, 确证比对时, 除要保证被测样和标准物质的试验参数如碰撞能量等参数一致外, 还应选择与样品中可疑化合物浓度相当的标准溶液进行比对, 从而增加确证的可信度, 减少出现假阳性的概率。另外, 在无化合物对照品的情况下, 将样品中可疑化合物生成的二级质谱图与EPI数据谱库中的二级质谱图进行比对, 可实现对可疑非法添加药物的初步鉴定。
2.5 方法学考察
2.5.1 空白试验
除不加试样外, 按1.3.2样品制备项下操作制得空白溶液, 上机分析, 结果表明, 实验所用试剂耗材和方法对15种化学药物的检测均无干扰。
2.5.2 线性范围和检出限
将用复溶溶剂配制的系列混合标准工作溶液上机测定, 外标法定量, 以化合物的浓度对峰面积进行线性回归, 得到各化合物的回归方程和相关系数。结果(表2)表明, 15种化合物的线性相关系数范围为0.9956~0.9996, 均大于0.99, 线性良好。在空白样品中添加适量的一定浓度的混合标准溶液, 按本法处理后分析, 以3倍信噪比计算各目标化合物的检出限, 检出限范围为0.62~62.50 μg/kg。
2.5.3 精密度和回收率
称取2.00 g空白样品共18份, 每种化合物分别添加3个水平的加标量, 按本法处理和分析, 每个水平平行测定6次, 计算回收率和精密度。如表3所示, 各化合物的回收率范围为78.33%~109.51%, RSDs范围为0.67%~14.02%, 具有较好的准确度和精密度。
2.5.4 实际样品的测定
采用本研究建立的方法对温州地区45批次预制菜样品进行检测, 结果15批炖卤肉制品中有4批检出咖啡因, 分别为44.6、103.0、92.5、124.0 μg/kg, 有1批检出对乙酰氨基酚39.0 μg/kg, 其余样品均未检出。运用上述方法在获得可靠的定量结果的同时, 对阳性样品检出成分的二级质谱图和标准物质的二级质谱图进行比对, 匹配度均大于70%, 说明本方法对样品中目标物的EPI定性分析可信度较高。
3 结论
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本研究采用超高效液相色谱三重四极杆复合线性离子阱质谱法的MRM-IDA-EPI扫描方式建立了同时分析预制菜中15种化学药物的定性和定量方法。与传统的MRM模式相比, 有效降低了出现假阳性的概率。经优化质谱、前处理、色谱等条件后, 前处理易于操作, 15种目标化合物分离度好, 峰形尖锐, 结果准确可靠, 有较高的回收率, 可应用于预制菜中15种非法添加化学药物的定性筛查和定量分析。本研究有助于强化预制菜食品安全监管, 促进预制菜产业健康发展, 保障人民群众食品安全, 为预制菜相关检测标准的制定提供参考依据。
基金
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  • 浙江省市场监督管理局雏鹰计划核心项目(CY2022227)
  • 温州市市场监督管理局科技计划项目(2024006)
文献
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2025年第16卷第1期
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20241023003
  • 接收时间：2024-10-23
  • 首发时间：2025-07-21
  • 出版时间：2025-01-15
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  • 收稿日期：2024-10-23
基金
浙江省市场监督管理局雏鹰计划核心项目(CY2022227)
温州市市场监督管理局科技计划项目(2024006)
作者信息
    温州市食品药品检验科学研究院, 温州 325000

通讯作者:

*李志梅(1975—), 女, 副主任药师, 主要研究方向为食品、药品仪器分析检测。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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