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Article(id=1248601954910359570, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1248601950581842932, articleNumber=1001-2494(2024)08-0694-09, orderNo=null, doi=null, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1677772800000, receivedDateStr=2023-03-03, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1775619503952, onlineDateStr=2026-04-08, pubDate=1713715200000, pubDateStr=2024-04-22, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1775619503952, onlineIssueDateStr=2026-04-08, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1775619503952, creator=13701087609, updateTime=1775619503952, updator=13701087609, issue=Issue{id=1248601950581842932, tenantId=1146029695717560320, journalId=1190317699101192196, year='2024', volume='59', issue='8', pageStart='657', pageEnd='754', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1775619502920, creator=13701087609, updateTime=1775620003727, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1248604051202527794, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1248601950581842932, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1248604051202527795, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1248601950581842932, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=694, endPage=702, ext={EN=ArticleExt(id=1248601955216543779, articleId=1248601954910359570, tenantId=1146029695717560320, journalId=1190317699101192196, language=EN, title=Determination and Preliminary Risk Assessment of 18 Polycyclic Aromatic Hydrocarbons in Seed-Fruit Herbs by Molecular Imprinting Solid Phase Extraction Combined with Gas Chromatography-Mass Spectrometry, columnId=null, journalTitle=Chinese Pharmaceutical Journal, columnName=null, runingTitle=null, highlight=null, articleAbstract=

OBJECTIVE To research and evaluate risk of 18 polycyclic aromatic hydrocarbons(PAHs) in seed-fruit herbs based on a SPE-isotope dilution GC-MS/MS method for the determination of the residues. METHODS Using isotope as internal standard, the sample was extracted by n-hexane and purified by molecular imprinting solid phase extraction. GC-MS /MS method was used for the assay. The chromatographic column was DB-17ms(0.25 mm×30 m, 0.25 μm) with temperature programming and MRM detection. The preliminary risk assessment of polycyclic aromatic hydrocarbons (PAHs) in seeds and fruits of traditional Chinese medicine (TCM) was carried out by using toxicity equivalent factor method. RESULTS The calibration curves for the 18 kinds of typical PAHs were linear in the range of 2-50 ng·mL-1. The average recovery rate was in the range of 77.25%-112.32%, with RSD 2.74%-15.89% (n=3). The LOQs were 0.2-1 μg·kg-1 According to the risk assessment results, some varieties may have potential cancer risk. CONCLUSION This method is specific, sensitive, and can be used for residue detection of 18 typical kinds of PAHs in seed-fruit herbs. The residual amount of PAHs in some seeds and fruits of traditional Chinese medicine may have a potential cancer risk, which need attention.

, correspAuthors=Ke ZAN, Hongyu JIN, 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=Lina LIU, Tiantian ZUO, Ke ZAN, Hongyu JIN, Shuangcheng MA), CN=ArticleExt(id=1248601959448596725, articleId=1248601954910359570, tenantId=1146029695717560320, journalId=1190317699101192196, language=CN, title=分子印迹固相萃取-同位素内标-GC-MS/MS法测定种子果实类中药材中18种多环芳烃残留量及其初步风险评估, columnId=1190352405612040510, journalTitle=中国药学杂志, columnName=论著, runingTitle=null, highlight=null, articleAbstract=

目的 建立了分子印迹固相萃取-同位素内标-气相色谱质谱联用(GC-MS/MS)法测定种子果实类中药材中18种多环芳烃的残留量的方法,并对其进行初步风险评估,为评价种子果实类中药材安全性提供有效分析手段。方法 采用氘代多环芳烃同位素内标,样品以正己烷提取,经分子印迹固相萃取小柱净化后,采用GC-MS/MS法测定,色谱柱为DM-17ms(0.25 mm×30 m,0.25 μm),程序升温,以多反应离子监测模式进行检测。采用毒性当量因子法对种子果实类中药材中多环芳烃进行初步风险评估。结果 18种多环芳烃在2~50 ng·mL-1内线性关系良好;在2~50 μg·kg-1内的平均回收率为77.25%~112.32%,相对标准偏差(RSD)为2.74%~15.89% (n=3);方法定量限为0.2~1 μg·kg-1。根据风险评估结果,部分品种ILCR值介于10-4与10-6之间。结论 本方法操作简便、专属性强、灵敏度高,可满足种子果实类中药材中18种多环芳烃残留的定量检测工作。部分种子果实类中药多环芳烃残留量可能存在潜在致癌风险,需要引起注意。

, correspAuthors=昝珂, 金红宇, authorNote=null, correspAuthorsNote=
*昝珂,男,副研究员 研究方向:中药、天然药质量控制及内源性有害物质研究 Tel:(010)53852092;
金红宇,男,主任药师 研究方向:中药、天然药质量控制及有害残留物分析 Tel:(010)53852076
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刘丽娜,女,副研究员 研究方向:中药、天然药质量控制及有害残留物分析

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刘丽娜,女,副研究员 研究方向:中药、天然药质量控制及有害残留物分析

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刘丽娜,女,副研究员 研究方向:中药、天然药质量控制及有害残留物分析

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DOI:10.1016/j.jhazmat.2021.126708., articleTitle=Assessment of polycyclic aromatic hydrocarbons in seafood collected from coastal aquaculture ponds in Taiwan and human health risk assessment, refAbstract=null), Reference(id=1249073253050950182, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, doi=null, pmid=null, pmcid=null, year=2017, volume=37, issue=12, pageStart=4772, pageEnd=4778, url=null, language=null, rfNumber=[18], rfOrder=17, authorNames=WEI G E, CHENG Q, CHAI C, journalName=Acta Sci Circumst, refType=null, unstructuredReference=WEI G E, CHENG Q, CHAI C, et al. Characteristics of pollution and health risk assessment of polycyclic aromatic hydrocarbons in vegetables from Qingdao suburb[J]. Acta Sci Circumst, 2017, 37(12): 4772-4778., articleTitle=Characteristics of pollution and health risk assessment of polycyclic aromatic hydrocarbons in vegetables from Qingdao suburb, refAbstract=null)], funds=[Fund(id=1249073251247399408, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, awardId=GTTS-2022-7-2, language=CN, fundingSource=中国食品药品检定研究院关键技术研究基金项目资助(GTTS-2022-7-2), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1249073243622154569, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, xref=null, ext=[AuthorCompanyExt(id=1249073243634737482, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, companyId=1249073243622154569, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=National Institutes for Food and Drug Control, Beijing 102629, China), AuthorCompanyExt(id=1249073243643126091, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, companyId=1249073243622154569, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=中国食品药品检定研究院, 北京 102629)])], figs=[ArticleFig(id=1249073248168780222, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, language=EN, label=Tab.1, caption=

The information for 18 PAHs and isotopes

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Name Structure Formula Mr CAS TEF
1 Naphthalene(Naph) C10H8 128.17 91-20-3 0.001
2 Acenaphthylene(Acy) C12H8 152.19 208-96-8 0.001
3 Acenaphthene(Ace) C12H10 154.21 83-32-9 0.001
4 Fluorene(Flu) C13H10 166.22 86-73-7 0.001
5 Phenanthrene(Phe) C14H10 178.23 85-01-8 0001
6 Anthracene(Ant) C14H10 178.23 120-12-7 0.010
7 Fluoranthene(Flt) C16H10 202.25 206-44-0 0.001
8 Pyrene(Pry) C16H10 202.25 129-00-0 0.001
9 Benzo(a) anthracene(Baa) C18H12 228.29 56-55-3 0.100
10 Chrysene(Chry) C18H12 228.29 218-01-9 0.01
11 Benzo(b) fluoranthene(Bbf) C22H12 252.31 205-99-2 0.100
12 Benzo(k) fluoranthene(Bkf) C2C22H12 252.31 207-08-9 0.100
13 Benzo(j) fluoranthene(Bjf) C2C22H12 252.31 205-910-3 -
14 Benzo(e) pyrene(Bep) C2C22H12 252.31 205-99-2 -
15 Benzo(a) pyrene(Bap) C20H12 252.31 50-32-8 1.000
16 Indeno(1,2,3-cd) pyrene(Indp) C22H12 276.33 193-39-5 0.100
17 Dibenzo(a,h) anthracene(Dbaha) C22H14 278.35 200-181-8 1.000
18 Benzo(ghi) perylene(Bghip) C22H12 276.33 191-24-2 0.010
), ArticleFig(id=1249073248256860609, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, language=CN, label=表1, caption=

18种多环芳烃及其同位素内标的信息表

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Name Structure Formula Mr CAS TEF
1 Naphthalene(Naph) C10H8 128.17 91-20-3 0.001
2 Acenaphthylene(Acy) C12H8 152.19 208-96-8 0.001
3 Acenaphthene(Ace) C12H10 154.21 83-32-9 0.001
4 Fluorene(Flu) C13H10 166.22 86-73-7 0.001
5 Phenanthrene(Phe) C14H10 178.23 85-01-8 0001
6 Anthracene(Ant) C14H10 178.23 120-12-7 0.010
7 Fluoranthene(Flt) C16H10 202.25 206-44-0 0.001
8 Pyrene(Pry) C16H10 202.25 129-00-0 0.001
9 Benzo(a) anthracene(Baa) C18H12 228.29 56-55-3 0.100
10 Chrysene(Chry) C18H12 228.29 218-01-9 0.01
11 Benzo(b) fluoranthene(Bbf) C22H12 252.31 205-99-2 0.100
12 Benzo(k) fluoranthene(Bkf) C2C22H12 252.31 207-08-9 0.100
13 Benzo(j) fluoranthene(Bjf) C2C22H12 252.31 205-910-3 -
14 Benzo(e) pyrene(Bep) C2C22H12 252.31 205-99-2 -
15 Benzo(a) pyrene(Bap) C20H12 252.31 50-32-8 1.000
16 Indeno(1,2,3-cd) pyrene(Indp) C22H12 276.33 193-39-5 0.100
17 Dibenzo(a,h) anthracene(Dbaha) C22H14 278.35 200-181-8 1.000
18 Benzo(ghi) perylene(Bghip) C22H12 276.33 191-24-2 0.010
), ArticleFig(id=1249073248357523909, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, language=EN, label=Tab.2, caption=

The retention time and the mass spectrum conditions for MS detection of 18 PAHs

, figureFileSmall=null, figureFileBig=null, tableContent=
Name Retention
time/min		 Quantifier
transition 1		 Collision
energy/eV		 Ion pair 1 for
qualitative analysis		 Collision
energy/eV		 Ion pair 2 for
qualitative analysis		 Collision
energy/eV
Naph 4.07 128.10>102.10 20 128.10>127.10 15 128.10>77.10 20
Naph-d8 4.04 136.10>108.10 25 136.10>134.10 20
Acy 7.15 152.10>151.10 15 152.10>126.10 20 152.10>150.10 15
Acy-d8 7.11 160.10>158.10 15 160.10>132.10 30
Ace 7.42 154.10>151.10 35 154.10>152.10 30 154.10>153.10 10
Ace-d10 7.34 164.20>162.20 10 164.20>160.20 30
Flu 8.56 166.10>165.10 25 166.10>164.10 25
Flu-d10 8.48 176.20>174.20 15 176.20>175.20 15
Phe 10.93 178.10>176.10 30 178.10>152.10 25 178.10>177.10 25
Phe-d10 10.88 188.20>160.20 25 188.20>184.20 25 0.00>0.00 0
Ant 11.00 178.10>176.10 30 178.10>152.10 25 178.10>177.10 25
Ant-d10 10.96 188.20>160.20 25 188.20>184.20 25
Flt-d10 13.00 212.20>208.20 30 212.20>210.20 25
Pyr-d10 13.52 212.20>208.20 30 212.20>210.20 25
Flt 13.04 202.10>200.10 30 202.10>201.40 15 202.10>152.10 30
Pyr 13.56 202.10>200.10 30 202.10>201.40 15 202.10>152.10 30
Baa 16.57 228.10>226.10 25 228.10>202.10 20 228.10>227.10 20
Chry 16.84 228.10>226.10 25 228.10>202.10 20 228.10>227.10 20
Baa-d12 16.49 240.20>236.20 30 240.20>212.20 20
Chry-d12 16.74 240.20>236.20 30 240.20>212.20 20
Bbf 20.90 252.10>250.10 35 252.10>224.10 50 252.10>251.10 15
Bkf 21.02 252.10>250.10 35 252.10>224.10 50 252.10>251.10 15
Bjf 21.14 252.10>250.10 35 252.10>224.10 50 252.10>251.10 15
Bbf-d12 20.78 264.20>260.20 30 264.20>232.20 50
Bkf-d12 20.91 264.20>260.20 30 264.20>232.20 50
Bep 22.57 252.10>250.10 35 252.10>224.10 50 252.10>251.10 15
Bap 22.83 252.10>250.10 35 252.10>224.10 50 252.10>251.10 15
Bap-d12 22.69 264.20>260.20 30 264.20>232.20 50
Indp 29.49 276.10>274.10 30 276.10>275.10 40 276.10>276.10 20
Dbaha 29.60 278.10>276.10 30 278.10>277.10 25 278.10>278.10 20
Indp-d12 29.40 288.20>284.20 30 288.20>287.20 10
Dbaha-d14 29.42 292.20>288.20 30 292.20>291.20 20
Bghip 30.88 276.10>274.10 30 276.10>275.10 25
Bghip-d12 30.75 288.20>284.20 30 288.20>286.20 30
), ArticleFig(id=1249073248466575817, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, language=CN, label=表2, caption=

18种多环芳烃及相应同位素内标物保留时间及定量、定性离子

, figureFileSmall=null, figureFileBig=null, tableContent=
Name Retention
time/min		 Quantifier
transition 1		 Collision
energy/eV		 Ion pair 1 for
qualitative analysis		 Collision
energy/eV		 Ion pair 2 for
qualitative analysis		 Collision
energy/eV
Naph 4.07 128.10>102.10 20 128.10>127.10 15 128.10>77.10 20
Naph-d8 4.04 136.10>108.10 25 136.10>134.10 20
Acy 7.15 152.10>151.10 15 152.10>126.10 20 152.10>150.10 15
Acy-d8 7.11 160.10>158.10 15 160.10>132.10 30
Ace 7.42 154.10>151.10 35 154.10>152.10 30 154.10>153.10 10
Ace-d10 7.34 164.20>162.20 10 164.20>160.20 30
Flu 8.56 166.10>165.10 25 166.10>164.10 25
Flu-d10 8.48 176.20>174.20 15 176.20>175.20 15
Phe 10.93 178.10>176.10 30 178.10>152.10 25 178.10>177.10 25
Phe-d10 10.88 188.20>160.20 25 188.20>184.20 25 0.00>0.00 0
Ant 11.00 178.10>176.10 30 178.10>152.10 25 178.10>177.10 25
Ant-d10 10.96 188.20>160.20 25 188.20>184.20 25
Flt-d10 13.00 212.20>208.20 30 212.20>210.20 25
Pyr-d10 13.52 212.20>208.20 30 212.20>210.20 25
Flt 13.04 202.10>200.10 30 202.10>201.40 15 202.10>152.10 30
Pyr 13.56 202.10>200.10 30 202.10>201.40 15 202.10>152.10 30
Baa 16.57 228.10>226.10 25 228.10>202.10 20 228.10>227.10 20
Chry 16.84 228.10>226.10 25 228.10>202.10 20 228.10>227.10 20
Baa-d12 16.49 240.20>236.20 30 240.20>212.20 20
Chry-d12 16.74 240.20>236.20 30 240.20>212.20 20
Bbf 20.90 252.10>250.10 35 252.10>224.10 50 252.10>251.10 15
Bkf 21.02 252.10>250.10 35 252.10>224.10 50 252.10>251.10 15
Bjf 21.14 252.10>250.10 35 252.10>224.10 50 252.10>251.10 15
Bbf-d12 20.78 264.20>260.20 30 264.20>232.20 50
Bkf-d12 20.91 264.20>260.20 30 264.20>232.20 50
Bep 22.57 252.10>250.10 35 252.10>224.10 50 252.10>251.10 15
Bap 22.83 252.10>250.10 35 252.10>224.10 50 252.10>251.10 15
Bap-d12 22.69 264.20>260.20 30 264.20>232.20 50
Indp 29.49 276.10>274.10 30 276.10>275.10 40 276.10>276.10 20
Dbaha 29.60 278.10>276.10 30 278.10>277.10 25 278.10>278.10 20
Indp-d12 29.40 288.20>284.20 30 288.20>287.20 10
Dbaha-d14 29.42 292.20>288.20 30 292.20>291.20 20
Bghip 30.88 276.10>274.10 30 276.10>275.10 25
Bghip-d12 30.75 288.20>284.20 30 288.20>286.20 30
), ArticleFig(id=1249073248575627725, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, language=EN, label=Tab.3, caption=

Regressive equations,correlation coefficients,linear ranges,precision and detection limits for 18 PAHs

, figureFileSmall=null, figureFileBig=null, tableContent=
Name Standard curve r LOD/μg·kg-1 Precision,RSD/%
Naph Y=0.977X+0.757 1.000 0.800 6.52
Acy Y=0.182X+0.051 1.000 0.200 6.93
Ace Y=2.881X+0.927 1.000 1.000 8.53
Flu Y=1.484X+0.990 1.000 1.000 5.04
Phe Y=1.782X+1.372 1.000 0.500 7.35
Ant Y=2.061X+0.331 1.000 0.200 4.62
Flt Y=3.236X+1.024 1.000 1.000 6.13
Pyr Y=2.459X+0.865 1.000 1.000 3.51
Baa Y=2.104X+0.348 1.000 1.000 3.90
Chry Y=2.180X+0.423 1.000 1.000 2.86
Bbf Y=2.028X+0.433 1.000 0.800 7.33
Bkf Y=2.100X+0.370 1.000 0.800 6.94
Bjf Y=2.197X+0.430 1.000 0.800 3.77
Bep Y=2.891X+0.847 1.000 0.200 3.62
Bap Y=1.854X+0.295 1.000 0.800 6.52
Indp Y=2.688X-0.244 1.000 0.700 5.39
Dbaha Y=1.332X+0.367 1.000 0.500 6.67
Bghip Y=3.309X+0.733 1.000 0.300 5.83
), ArticleFig(id=1249073248642736591, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, language=CN, label=表3, caption=

18种多环芳烃的线性及范围、灵敏度及精密度

, figureFileSmall=null, figureFileBig=null, tableContent=
Name Standard curve r LOD/μg·kg-1 Precision,RSD/%
Naph Y=0.977X+0.757 1.000 0.800 6.52
Acy Y=0.182X+0.051 1.000 0.200 6.93
Ace Y=2.881X+0.927 1.000 1.000 8.53
Flu Y=1.484X+0.990 1.000 1.000 5.04
Phe Y=1.782X+1.372 1.000 0.500 7.35
Ant Y=2.061X+0.331 1.000 0.200 4.62
Flt Y=3.236X+1.024 1.000 1.000 6.13
Pyr Y=2.459X+0.865 1.000 1.000 3.51
Baa Y=2.104X+0.348 1.000 1.000 3.90
Chry Y=2.180X+0.423 1.000 1.000 2.86
Bbf Y=2.028X+0.433 1.000 0.800 7.33
Bkf Y=2.100X+0.370 1.000 0.800 6.94
Bjf Y=2.197X+0.430 1.000 0.800 3.77
Bep Y=2.891X+0.847 1.000 0.200 3.62
Bap Y=1.854X+0.295 1.000 0.800 6.52
Indp Y=2.688X-0.244 1.000 0.700 5.39
Dbaha Y=1.332X+0.367 1.000 0.500 6.67
Bghip Y=3.309X+0.733 1.000 0.300 5.83
), ArticleFig(id=1249073248735011281, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, language=EN, label=Tab.4, caption=

Repeatability results of PAHs

, figureFileSmall=null, figureFileBig=null, tableContent=
Name 1 2 3 4 5 6 Average RSD/%
Naph - - - - - - - -
Ace 0.32 0.38 0.38 0.38 0.42 0.37 0.37 8.29
Flu 4.48 4.30 4.36 5.48 4.49 4.53 4.61 9.52
Phe 23.60 23.19 20.30 21.23 23.25 22.15 22.29 5.86
Ant 4.03 4.02 3.43 4.13 4.21 3.84 3.94 7.05
Flt 5.04 4.80 4.37 4.89 5.05 4.65 4.80 5.43
Pyr 3.35 3.69 3.48 3.52 3.16 3.04 3.37 7.18
Baa - - - - - - - -
Chry - - - - - - - -
Bbf - - - - - - - -
Bkf - - - - - - - -
Bjf - - - - - - - -
Bep - - - - - - - -
Bap - - - - - - - -
Indp - - - - - - - -
Dbaha - - - - - - - -
Bghip - - - - - - - -
), ArticleFig(id=1249073248814703061, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, language=CN, label=表4, caption=

多环芳烃检测重复性结果

, figureFileSmall=null, figureFileBig=null, tableContent=
Name 1 2 3 4 5 6 Average RSD/%
Naph - - - - - - - -
Ace 0.32 0.38 0.38 0.38 0.42 0.37 0.37 8.29
Flu 4.48 4.30 4.36 5.48 4.49 4.53 4.61 9.52
Phe 23.60 23.19 20.30 21.23 23.25 22.15 22.29 5.86
Ant 4.03 4.02 3.43 4.13 4.21 3.84 3.94 7.05
Flt 5.04 4.80 4.37 4.89 5.05 4.65 4.80 5.43
Pyr 3.35 3.69 3.48 3.52 3.16 3.04 3.37 7.18
Baa - - - - - - - -
Chry - - - - - - - -
Bbf - - - - - - - -
Bkf - - - - - - - -
Bjf - - - - - - - -
Bep - - - - - - - -
Bap - - - - - - - -
Indp - - - - - - - -
Dbaha - - - - - - - -
Bghip - - - - - - - -
), ArticleFig(id=1249073248890200537, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, language=EN, label=Tab.5, caption=

Average recoveries and RSDs of polycyclic aromatic hydrocarbons. n=3

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Name 2 μg·kg-1 5 μg·kg-1 50 μg·kg-1
Recovery
/%		 RSD
/%		 Recovery
/%		 RSD
/%		 Recovery
/%		 RSD
/%
1 Naph 89.78 11.22 85.44 4.77 117.67 5.51
2 Acy 85.24 2.74 99.64 8.10 102.36 12.08
3 Ace 109.14 3.27 102.23 6.58 93.75 4.79
4 Flu 84.42 10.44 107.03 4.90 100.77 5.25
5 Phe 77.25 13.04 83.07 10.33 89.80 1.79
6 Ant 99.92 3.50 93.88 13.57 90.35 3.85
7 Flt 87.17 15.48 86.34 11.56 96.34 2.02
8 Pyr 107.08 15.89 104.84 3.99 95.56 0.53
9 Baa 110.43 4.40 96.03 8.47 97.51 5.45
10 Chry 82.27 4.93 91.59 4.85 99.08 3.95
11 Bbf 111.55 5.04 112.32 4.05 89.65 6.99
12 Bkf 89.61 12.04 94.39 8.62 110.96 3.82
13 Bjf 80.84 9.14 96.46 3.75 109.52 4.23
14 Bep 95.29 5.70 100.45 12.52 98.03 9.34
15 Bap 93.87 5.10 102.47 7.24 101.31 7.72
16 Indp 82.07 8.81 92.35 9.54 104.62 6.10
17 Dbaha 87.98 5.15 87.64 12.71 97.91 8.40
18 Bghip 102.03 5.78 106.53 7.16 99.14 5.04
), ArticleFig(id=1249073248978280921, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, language=CN, label=表5, caption=

18种多环芳烃的三水平回收率. n=3

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Name 2 μg·kg-1 5 μg·kg-1 50 μg·kg-1
Recovery
/%		 RSD
/%		 Recovery
/%		 RSD
/%		 Recovery
/%		 RSD
/%
1 Naph 89.78 11.22 85.44 4.77 117.67 5.51
2 Acy 85.24 2.74 99.64 8.10 102.36 12.08
3 Ace 109.14 3.27 102.23 6.58 93.75 4.79
4 Flu 84.42 10.44 107.03 4.90 100.77 5.25
5 Phe 77.25 13.04 83.07 10.33 89.80 1.79
6 Ant 99.92 3.50 93.88 13.57 90.35 3.85
7 Flt 87.17 15.48 86.34 11.56 96.34 2.02
8 Pyr 107.08 15.89 104.84 3.99 95.56 0.53
9 Baa 110.43 4.40 96.03 8.47 97.51 5.45
10 Chry 82.27 4.93 91.59 4.85 99.08 3.95
11 Bbf 111.55 5.04 112.32 4.05 89.65 6.99
12 Bkf 89.61 12.04 94.39 8.62 110.96 3.82
13 Bjf 80.84 9.14 96.46 3.75 109.52 4.23
14 Bep 95.29 5.70 100.45 12.52 98.03 9.34
15 Bap 93.87 5.10 102.47 7.24 101.31 7.72
16 Indp 82.07 8.81 92.35 9.54 104.62 6.10
17 Dbaha 87.98 5.15 87.64 12.71 97.91 8.40
18 Bghip 102.03 5.78 106.53 7.16 99.14 5.04
), ArticleFig(id=1249073249087332828, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, language=EN, label=Tab.6, caption=

Residues of PAHs found in root and rhizome herbs. n=42

, figureFileSmall=null, figureFileBig=null, tableContent=
Name Content/μg·kg-1 Detection
rate/%
Range $\stackrel{-}{x}$±s
Naph 14.7 -906.8 247.8 ±176.1 100
Acy 0.0 -21.0 3.3 ±5.4 54
Ace 0 -6.5 1.3 ±1.8 57
Flu 0.0 -164.8 21.5 ±27.1 97
Phe 12.2 -1 866.2 153.7 ±310.4 100
Ant 0.0 -165.2 15.9 ±27.7 95
Flt 1.4 -1 778.6 114.4 ±305.5 100
Pyr 1.4 -1 635.1 101.6 ±276.6 100
Baa 0.0 -250.5 23.8 ±50.8 92
Chry 0.0 -256.4 26.7 ±56.8 70
Bbf 0.0 -64.3 7.4 ±14.4 73
Bkf 0.0 -1 821.3 52.2 ±299.0 76
Bjf 0.0 -2 491.6 71.0 ±409.1 51
Bep 0.0 -27.7 3.6 ±6.3 65
Bap 0.0 -43.9 4.6 ±9.3 65
Indp 0.0 -18.1 2.3 ±4.2 81
Dbaha 0.0 -9.0 0.6 ±1.8 32
Bghip 0.0 -34.9 3.4 ±7.5 46
∑LPAHs 50.5 -5 061.1 709.9 ±972.3 100
∑HPAHs 0.0 -4 333.0 145.0 ±710.0 92
∑2PAHs 0.0 -300.3 31.3 ±65.9 76
∑4PAHs 0.3 -615.1 62.5 ±130.7 100
∑8PAHs 0.4 -1 866.1 121.0 ±331.1 100
∑18PAHs 117.5 -11 553.0 1.803.5 ±2.615.2 100
), ArticleFig(id=1249073249167024607, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, language=CN, label=表6, caption=

种子果实类中药多环芳烃污染情况汇总. n=42

, figureFileSmall=null, figureFileBig=null, tableContent=
Name Content/μg·kg-1 Detection
rate/%
Range $\stackrel{-}{x}$±s
Naph 14.7 -906.8 247.8 ±176.1 100
Acy 0.0 -21.0 3.3 ±5.4 54
Ace 0 -6.5 1.3 ±1.8 57
Flu 0.0 -164.8 21.5 ±27.1 97
Phe 12.2 -1 866.2 153.7 ±310.4 100
Ant 0.0 -165.2 15.9 ±27.7 95
Flt 1.4 -1 778.6 114.4 ±305.5 100
Pyr 1.4 -1 635.1 101.6 ±276.6 100
Baa 0.0 -250.5 23.8 ±50.8 92
Chry 0.0 -256.4 26.7 ±56.8 70
Bbf 0.0 -64.3 7.4 ±14.4 73
Bkf 0.0 -1 821.3 52.2 ±299.0 76
Bjf 0.0 -2 491.6 71.0 ±409.1 51
Bep 0.0 -27.7 3.6 ±6.3 65
Bap 0.0 -43.9 4.6 ±9.3 65
Indp 0.0 -18.1 2.3 ±4.2 81
Dbaha 0.0 -9.0 0.6 ±1.8 32
Bghip 0.0 -34.9 3.4 ±7.5 46
∑LPAHs 50.5 -5 061.1 709.9 ±972.3 100
∑HPAHs 0.0 -4 333.0 145.0 ±710.0 92
∑2PAHs 0.0 -300.3 31.3 ±65.9 76
∑4PAHs 0.3 -615.1 62.5 ±130.7 100
∑8PAHs 0.4 -1 866.1 121.0 ±331.1 100
∑18PAHs 117.5 -11 553.0 1.803.5 ±2.615.2 100
), ArticleFig(id=1249073250752471522, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, language=EN, label=Tab.7, caption=

The average concentration of 18 PAHs in Root and rhizome herbs. μg·kg-1

, figureFileSmall=null, figureFileBig=null, tableContent=
Name Hordei Fructus
Germinatus(n=2)		 Fried Hordei
Fructus Germinatus		 Crataegi
Fructus		 Fried Crataegi
Fructus(n=1)		 Pericarpium
Citri Reticulatae		 Fructus
Gardeniae		 Fructus
Chaenomelis		 Fructus
Corni		 Chebulae
Fructus
Naph 279.0 ±71.1 336.21 309.6 ±79.5 238.39 236.6 ±91.2 301.4 ±43.4 170.1 ±67.8 573.2 ±399.4 259.38
Acy 4.8 ±5.7 2.10 4.2 ±1.0 15.18 1.6 ±0.2 16.7 ±4.5 5.2 ±5.7 - -
Ace 2.4 ±2.4 - 2.8 ±1.8 2.39 0.7 ±0.5 3.4 ±2.7 2.1 ±1.9 - 1.50
Flu 20.8 ±6.4 20.40 26.0 ±2.5 43.97 4.6 ±3.1 38.2 ±4.8 8.5 ±4.5 10.2 ±3.1 22.83
Phe 61.3 ±16.5 52.58 157.6 ±62.7 675.32 57.4 ±15.7 158.2 ±19.9 45.0 ±7.2 138.6 ±45.8 187.36
Ant 1.4 ±2.6 6.20 31.3 ±20.5 165.19 7.4 ±3.1 26.0 ±9.9 4.6 ±1.1 25.9 ±1.5 -
Flt 4.9 ±1.9 6.62 121.3 ±73.9 1 778.57 44.9 ±12.8 209.1 ±124.3 7.4 ±1.6 104.6 ±51.2 20.57
Pyr 2.2 ±1.1 4.14 94.3 ±59.1 1 635.14 40.2 ±9.4 205.7 ±132.8 5.5 ±1.2 92.6 ±51.0 21.69
Baa 1.0 ±0.8 - 11.8 ±2.7 250.51 11.7 ±1.3 61.5 ±45.0 3.9 ±2.5 23.9 ±11.1 -
Chry - - 19.2 ±2.8 256.41 15.3 ±0.2 64.1 ±42.3 - 30.8 ±13.3 -
Bbf - 0.31 3.0 ±0.5 64.29 5.3 ±3.1 19.0 ±15.0 0.6 ±1.0 8.6 ±3.9 1.78
Bkf - - - 30.37 608.4 ±1 050.4 9.8 ±8.5 - 3.3 ±2.2 -
Bjf - - 0.1 ±0.9 33.96 832.5 ±1 436.8 10.8 ±9.4 0.1 ±0.2 4.7 ±3.2 0.18
Bep - - 0.9 ±0.3 25.67 3.9 ±0.9 5.4 ±7.5 - 5.5 ±2.2 1.06
Bap - - 0.5 ±0.2 43.89 3.7 ±0.3 10.9 ±9.5 0.1 ±0.1 6.0 ±3.4 -
Indp - 0.21 0.3 ±0.3 17.96 2.0 ±0.2 3.9 ±3.3 0.1 ±0.3 2.6 ±0.7 0.58
Dbaha - - - 6.65 - 0.9 ±1.3 - 0.4 ±0.4 -
Bghip - - - 34.94 4.1 ±0.9 7.5 ±6.7 - 4.1 ±2.7 -
∑LPAHs 377.9 ±90.9 428.25 778.0 ±302.0 5061.05 420.4 ±106.5 1 084.2 ±380.3 252.3 ±80.9 999.8 ±380.0 513.33
∑HPAHs - 0.52 4.8 ±1.0 257.73 1 459.9 ±2 488.2 66.0 ±56.4 1.0 ±1.6 35.3 ±18.2 3.59
∑2PAHs - - 19.8 ±2.6 300.29 19.0 ±0.4 75.0 ±51.8 0.1 ±0.1 36.8 ±16.6 0.00
∑4PAHs 1.0 ±0.8 0.31 34.6 ±5.4 615.09 36.0 ±4.2 155.4 ±111.4 4.5 ±3.4 69.3 ±31.5 1.78
∑8PAHs 3.4 ±3.3 0.52 18.4 ±1.5 450.99 635.8 ±1 052.3 116.5 ±85.7 6.8 ±5.2 48.9 ±24.0 3.85
∑18PAHs 377.9 ±90.9 428.77 782.8 ±301.2 5318.79 1 880.3 ±2 570.9 1 150.3 ±436.1 253.2 ±81.4 1 035.1 ±379.0 516.92
Name Fructus
Momordicae		 Semen
Coicis		 Fructus Mume
(n=2)		 Fructus Mume
Carbon(n=1)		 Mori
Fructus		 Fired Semen Lablab
Album(n=2)		 Semen Lablab
Album(n=1)		 Bran fried Fructus
Aurantii Immaturus
Naph 218.6 ±53.4 189.24 241.1 ±67.2 192.21 319.9 ±244.2 113.7 ±45.4 158.05 41.4 ±25.2
Acy - - - - - - - 2.6 ±1.3
Ace - 4.30 - - - - - 2.3 ±2.2
Flu 11.0 ±1.0 27.07 34.6 ±8.5 164.82 15.9 ±15.5 10.5 ±6.7 18.56 6.0 ±1.0
Phe 29.6 ±3.6 126.25 113.1 ±22.3 1866.25 103.9 ±77.9 89.3 ±37.4 113.20 18.1 ±3.3
Ant 5.1 ±2.6 2.34 9.4 ±4.1 3.89 8.6 ±6.8 13.1 ±12.9 11.67 7.0 ±0.6
Flt 15.6 ±1.5 7.49 16.1 ±20.5 637.61 39.3 ±31.9 23.7 ±31.5 19.01 14.8 ±1.0
Pyr 14.5 ±3.0 5.78 29.3 ±1.7 470.65 32.3 ±25.0 20.5 ±20.0 12.91 14.3 ±2.0
Baa 6.7 ±1.1 6.85 13.7 ±1.3 178.13 18.0 ±6.7 2.1 ±0.6 3.55 4.3 ±1.1
Chry 4.9 ±4.3 - 16.9 ±2.8 232.47 15.3 ±11.2 - 2.66 3.5 ±1.8
Bbf - - 2.8 ±0.6 56.09 6.1 ±5.2 - - 5.3 ±1.9
Bkf - - - 25.08 2.5 ±2.2 - - 1.2 ±2.1
Bjf - - 0.3 ±0.5 34.96 2.4 ±2.3 - - 1.1 ±1.9
Bep 1.2 ±1.2 - 1.2 ±0.5 27.71 4.2 ±4.1 - - 5.5 ±1.7
Bap 1.1 ±1.4 - 0.6 ±0.8 33.33 4.0 ±3.5 - - 4.4 ±1.7
Indp 0.7 ±0.9 0.29 0.3 ±0.4 18.12 2.0 ±1.5 3.0 ±4.2 0.11 1.9 ±1.0
Dbaha - - - 9.04 0.1 ±0.2 - - 1.3 ±0.2
Bghip 0.1 ±0.2 - - 28.60 2.7 ±2.6 - - 1.7 ±0.7
∑LPAHs 306.0 ±64.6 369.32 474.3 ±17.6 3 746.02 547.2 ±406.5 272.9 ±141.1 339.60 113.9 ±26.8
∑HPAHs 2.9 ±3.5 0.29 5.2 ±0.6 232.93 24.1 ±20.8 3.0 ±4.2 0.11 22.3 ±9.6
∑2PAHs 6.0 ±5.2 0.00 17.5 ±2.0 265.80 19.3 ±14.5 0.0 ±0.0 2.66 7.8 ±3.4
∑4PAHs 12.7 ±6.3 6.85 34.0 ±3.8 500.02 37.4 ±30.0 2.1 ±0.6 6.21 17.3 ±5.7
∑8PAHs 8.4 ±3.3 11.45 17.4 ±0.7 348.39 29.4 ±25.3 5.1 ±4.8 3.66 22.2 ±5.7
∑18PAHs 308.9 ±67.1 369.61 479.6 ±16.9 3 978.95 571.2 ±427.3 275.9 ±145.4 339.71 136.2 ±24.3
), ArticleFig(id=1249073250832163300, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, language=CN, label=表7, caption=

种子果实类样品中18种多环芳烃的平均浓度. μg·kg-1

, figureFileSmall=null, figureFileBig=null, tableContent=
Name Hordei Fructus
Germinatus(n=2)		 Fried Hordei
Fructus Germinatus		 Crataegi
Fructus		 Fried Crataegi
Fructus(n=1)		 Pericarpium
Citri Reticulatae		 Fructus
Gardeniae		 Fructus
Chaenomelis		 Fructus
Corni		 Chebulae
Fructus
Naph 279.0 ±71.1 336.21 309.6 ±79.5 238.39 236.6 ±91.2 301.4 ±43.4 170.1 ±67.8 573.2 ±399.4 259.38
Acy 4.8 ±5.7 2.10 4.2 ±1.0 15.18 1.6 ±0.2 16.7 ±4.5 5.2 ±5.7 - -
Ace 2.4 ±2.4 - 2.8 ±1.8 2.39 0.7 ±0.5 3.4 ±2.7 2.1 ±1.9 - 1.50
Flu 20.8 ±6.4 20.40 26.0 ±2.5 43.97 4.6 ±3.1 38.2 ±4.8 8.5 ±4.5 10.2 ±3.1 22.83
Phe 61.3 ±16.5 52.58 157.6 ±62.7 675.32 57.4 ±15.7 158.2 ±19.9 45.0 ±7.2 138.6 ±45.8 187.36
Ant 1.4 ±2.6 6.20 31.3 ±20.5 165.19 7.4 ±3.1 26.0 ±9.9 4.6 ±1.1 25.9 ±1.5 -
Flt 4.9 ±1.9 6.62 121.3 ±73.9 1 778.57 44.9 ±12.8 209.1 ±124.3 7.4 ±1.6 104.6 ±51.2 20.57
Pyr 2.2 ±1.1 4.14 94.3 ±59.1 1 635.14 40.2 ±9.4 205.7 ±132.8 5.5 ±1.2 92.6 ±51.0 21.69
Baa 1.0 ±0.8 - 11.8 ±2.7 250.51 11.7 ±1.3 61.5 ±45.0 3.9 ±2.5 23.9 ±11.1 -
Chry - - 19.2 ±2.8 256.41 15.3 ±0.2 64.1 ±42.3 - 30.8 ±13.3 -
Bbf - 0.31 3.0 ±0.5 64.29 5.3 ±3.1 19.0 ±15.0 0.6 ±1.0 8.6 ±3.9 1.78
Bkf - - - 30.37 608.4 ±1 050.4 9.8 ±8.5 - 3.3 ±2.2 -
Bjf - - 0.1 ±0.9 33.96 832.5 ±1 436.8 10.8 ±9.4 0.1 ±0.2 4.7 ±3.2 0.18
Bep - - 0.9 ±0.3 25.67 3.9 ±0.9 5.4 ±7.5 - 5.5 ±2.2 1.06
Bap - - 0.5 ±0.2 43.89 3.7 ±0.3 10.9 ±9.5 0.1 ±0.1 6.0 ±3.4 -
Indp - 0.21 0.3 ±0.3 17.96 2.0 ±0.2 3.9 ±3.3 0.1 ±0.3 2.6 ±0.7 0.58
Dbaha - - - 6.65 - 0.9 ±1.3 - 0.4 ±0.4 -
Bghip - - - 34.94 4.1 ±0.9 7.5 ±6.7 - 4.1 ±2.7 -
∑LPAHs 377.9 ±90.9 428.25 778.0 ±302.0 5061.05 420.4 ±106.5 1 084.2 ±380.3 252.3 ±80.9 999.8 ±380.0 513.33
∑HPAHs - 0.52 4.8 ±1.0 257.73 1 459.9 ±2 488.2 66.0 ±56.4 1.0 ±1.6 35.3 ±18.2 3.59
∑2PAHs - - 19.8 ±2.6 300.29 19.0 ±0.4 75.0 ±51.8 0.1 ±0.1 36.8 ±16.6 0.00
∑4PAHs 1.0 ±0.8 0.31 34.6 ±5.4 615.09 36.0 ±4.2 155.4 ±111.4 4.5 ±3.4 69.3 ±31.5 1.78
∑8PAHs 3.4 ±3.3 0.52 18.4 ±1.5 450.99 635.8 ±1 052.3 116.5 ±85.7 6.8 ±5.2 48.9 ±24.0 3.85
∑18PAHs 377.9 ±90.9 428.77 782.8 ±301.2 5318.79 1 880.3 ±2 570.9 1 150.3 ±436.1 253.2 ±81.4 1 035.1 ±379.0 516.92
Name Fructus
Momordicae		 Semen
Coicis		 Fructus Mume
(n=2)		 Fructus Mume
Carbon(n=1)		 Mori
Fructus		 Fired Semen Lablab
Album(n=2)		 Semen Lablab
Album(n=1)		 Bran fried Fructus
Aurantii Immaturus
Naph 218.6 ±53.4 189.24 241.1 ±67.2 192.21 319.9 ±244.2 113.7 ±45.4 158.05 41.4 ±25.2
Acy - - - - - - - 2.6 ±1.3
Ace - 4.30 - - - - - 2.3 ±2.2
Flu 11.0 ±1.0 27.07 34.6 ±8.5 164.82 15.9 ±15.5 10.5 ±6.7 18.56 6.0 ±1.0
Phe 29.6 ±3.6 126.25 113.1 ±22.3 1866.25 103.9 ±77.9 89.3 ±37.4 113.20 18.1 ±3.3
Ant 5.1 ±2.6 2.34 9.4 ±4.1 3.89 8.6 ±6.8 13.1 ±12.9 11.67 7.0 ±0.6
Flt 15.6 ±1.5 7.49 16.1 ±20.5 637.61 39.3 ±31.9 23.7 ±31.5 19.01 14.8 ±1.0
Pyr 14.5 ±3.0 5.78 29.3 ±1.7 470.65 32.3 ±25.0 20.5 ±20.0 12.91 14.3 ±2.0
Baa 6.7 ±1.1 6.85 13.7 ±1.3 178.13 18.0 ±6.7 2.1 ±0.6 3.55 4.3 ±1.1
Chry 4.9 ±4.3 - 16.9 ±2.8 232.47 15.3 ±11.2 - 2.66 3.5 ±1.8
Bbf - - 2.8 ±0.6 56.09 6.1 ±5.2 - - 5.3 ±1.9
Bkf - - - 25.08 2.5 ±2.2 - - 1.2 ±2.1
Bjf - - 0.3 ±0.5 34.96 2.4 ±2.3 - - 1.1 ±1.9
Bep 1.2 ±1.2 - 1.2 ±0.5 27.71 4.2 ±4.1 - - 5.5 ±1.7
Bap 1.1 ±1.4 - 0.6 ±0.8 33.33 4.0 ±3.5 - - 4.4 ±1.7
Indp 0.7 ±0.9 0.29 0.3 ±0.4 18.12 2.0 ±1.5 3.0 ±4.2 0.11 1.9 ±1.0
Dbaha - - - 9.04 0.1 ±0.2 - - 1.3 ±0.2
Bghip 0.1 ±0.2 - - 28.60 2.7 ±2.6 - - 1.7 ±0.7
∑LPAHs 306.0 ±64.6 369.32 474.3 ±17.6 3 746.02 547.2 ±406.5 272.9 ±141.1 339.60 113.9 ±26.8
∑HPAHs 2.9 ±3.5 0.29 5.2 ±0.6 232.93 24.1 ±20.8 3.0 ±4.2 0.11 22.3 ±9.6
∑2PAHs 6.0 ±5.2 0.00 17.5 ±2.0 265.80 19.3 ±14.5 0.0 ±0.0 2.66 7.8 ±3.4
∑4PAHs 12.7 ±6.3 6.85 34.0 ±3.8 500.02 37.4 ±30.0 2.1 ±0.6 6.21 17.3 ±5.7
∑8PAHs 8.4 ±3.3 11.45 17.4 ±0.7 348.39 29.4 ±25.3 5.1 ±4.8 3.66 22.2 ±5.7
∑18PAHs 308.9 ±67.1 369.61 479.6 ±16.9 3 978.95 571.2 ±427.3 275.9 ±145.4 339.71 136.2 ±24.3
), ArticleFig(id=1249073250949603815, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, language=EN, label=Tab.8, caption=

Preliminary risk assessment of polycyclic aromatic hydrocarbons in Chinese herbal medicines(×10-6)

, figureFileSmall=null, figureFileBig=null, tableContent=
Type Hordei Fructus
Germinatus
(n=2)		 Fried Hordei
Fructus
Germinatus		 Crataegi
Fructus		 Fried Crataegi
Fructus
(n=1)		 Pericarpium
Citri
Reticulatae		 Fructus
Gardeniae		 Fructus
Chaenomelis		 Fructus
Corni		 Chebulae
Fructus
ILCR 0.29 0.28 0.98 28.74 20.13 6.86 0.25 3.54 0.22
Type Fructus
Momordicae		 Semen
Coicis		 Fructus
Mume
(n=2)		 Fructus Mume
Carbon
(n=1)		 Mori
Fructus		 Fired Semen
Lablab Album
(n=2)		 Semen
Lablab
Album(n=1)		 Bran fried
Fructus Aurantii
Immaturus
ILCR 0.33 0.89 22.83 2.15 0.50 0.54 2.14 0.65
), ArticleFig(id=1249073251016712681, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1248601954910359570, language=CN, label=表8, caption=

中药材多环芳烃初步风险评估(×10-6)

, figureFileSmall=null, figureFileBig=null, tableContent=
Type Hordei Fructus
Germinatus
(n=2)		 Fried Hordei
Fructus
Germinatus		 Crataegi
Fructus		 Fried Crataegi
Fructus
(n=1)		 Pericarpium
Citri
Reticulatae		 Fructus
Gardeniae		 Fructus
Chaenomelis		 Fructus
Corni		 Chebulae
Fructus
ILCR 0.29 0.28 0.98 28.74 20.13 6.86 0.25 3.54 0.22
Type Fructus
Momordicae		 Semen
Coicis		 Fructus
Mume
(n=2)		 Fructus Mume
Carbon
(n=1)		 Mori
Fructus		 Fired Semen
Lablab Album
(n=2)		 Semen
Lablab
Album(n=1)		 Bran fried
Fructus Aurantii
Immaturus
ILCR 0.33 0.89 22.83 2.15 0.50 0.54 2.14 0.65
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分子印迹固相萃取-同位素内标-GC-MS/MS法测定种子果实类中药材中18种多环芳烃残留量及其初步风险评估
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刘丽娜 , 左甜甜 , 昝珂 * , 金红宇 * , 马双成
中国药学杂志 | 论著 2024,59(8): 694-702
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中国药学杂志 | 论著 2024, 59(8): 694-702
分子印迹固相萃取-同位素内标-GC-MS/MS法测定种子果实类中药材中18种多环芳烃残留量及其初步风险评估
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刘丽娜, 左甜甜, 昝珂*, 金红宇*, 马双成
作者信息
  • 中国食品药品检定研究院, 北京 102629

    • 刘丽娜,女,副研究员 研究方向:中药、天然药质量控制及有害残留物分析

通讯作者:

*昝珂,男,副研究员 研究方向:中药、天然药质量控制及内源性有害物质研究 Tel:(010)53852092;
金红宇,男,主任药师 研究方向:中药、天然药质量控制及有害残留物分析 Tel:(010)53852076
Determination and Preliminary Risk Assessment of 18 Polycyclic Aromatic Hydrocarbons in Seed-Fruit Herbs by Molecular Imprinting Solid Phase Extraction Combined with Gas Chromatography-Mass Spectrometry
Lina LIU, Tiantian ZUO, Ke ZAN*, Hongyu JIN*, Shuangcheng MA
Affiliations
  • National Institutes for Food and Drug Control, Beijing 102629, China
出版时间: 2024-04-22
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摘要
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目的 建立了分子印迹固相萃取-同位素内标-气相色谱质谱联用(GC-MS/MS)法测定种子果实类中药材中18种多环芳烃的残留量的方法,并对其进行初步风险评估,为评价种子果实类中药材安全性提供有效分析手段。方法 采用氘代多环芳烃同位素内标,样品以正己烷提取,经分子印迹固相萃取小柱净化后,采用GC-MS/MS法测定,色谱柱为DM-17ms(0.25 mm×30 m,0.25 μm),程序升温,以多反应离子监测模式进行检测。采用毒性当量因子法对种子果实类中药材中多环芳烃进行初步风险评估。结果 18种多环芳烃在2~50 ng·mL-1内线性关系良好;在2~50 μg·kg-1内的平均回收率为77.25%~112.32%,相对标准偏差(RSD)为2.74%~15.89% (n=3);方法定量限为0.2~1 μg·kg-1。根据风险评估结果,部分品种ILCR值介于10-4与10-6之间。结论 本方法操作简便、专属性强、灵敏度高,可满足种子果实类中药材中18种多环芳烃残留的定量检测工作。部分种子果实类中药多环芳烃残留量可能存在潜在致癌风险,需要引起注意。

多环芳烃  /  种子果实类中药  /  同位素内标  /  气相色谱质谱联用法  /  分子印迹固相萃取  /  风险评估

OBJECTIVE To research and evaluate risk of 18 polycyclic aromatic hydrocarbons(PAHs) in seed-fruit herbs based on a SPE-isotope dilution GC-MS/MS method for the determination of the residues. METHODS Using isotope as internal standard, the sample was extracted by n-hexane and purified by molecular imprinting solid phase extraction. GC-MS /MS method was used for the assay. The chromatographic column was DB-17ms(0.25 mm×30 m, 0.25 μm) with temperature programming and MRM detection. The preliminary risk assessment of polycyclic aromatic hydrocarbons (PAHs) in seeds and fruits of traditional Chinese medicine (TCM) was carried out by using toxicity equivalent factor method. RESULTS The calibration curves for the 18 kinds of typical PAHs were linear in the range of 2-50 ng·mL-1. The average recovery rate was in the range of 77.25%-112.32%, with RSD 2.74%-15.89% (n=3). The LOQs were 0.2-1 μg·kg-1 According to the risk assessment results, some varieties may have potential cancer risk. CONCLUSION This method is specific, sensitive, and can be used for residue detection of 18 typical kinds of PAHs in seed-fruit herbs. The residual amount of PAHs in some seeds and fruits of traditional Chinese medicine may have a potential cancer risk, which need attention.

polycyclic aromatic hydrocarbon  /  seed-fruit herb  /  isotope internal standard  /  GC-MS/MS  /  molecular imprinting solid phase extraction  /  risk assessment
刘丽娜, 左甜甜, 昝珂, 金红宇, 马双成. 分子印迹固相萃取-同位素内标-GC-MS/MS法测定种子果实类中药材中18种多环芳烃残留量及其初步风险评估. 中国药学杂志, 2024 , 59 (8) : 694 -702 .
Lina LIU, Tiantian ZUO, Ke ZAN, Hongyu JIN, Shuangcheng MA. Determination and Preliminary Risk Assessment of 18 Polycyclic Aromatic Hydrocarbons in Seed-Fruit Herbs by Molecular Imprinting Solid Phase Extraction Combined with Gas Chromatography-Mass Spectrometry[J]. Chinese Pharmaceutical Journal, 2024 , 59 (8) : 694 -702 .
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多环芳烃(polycyclic aromatic hydrocarbons,PAHs)是一类含有2个或2个以上苯环的化合物,许多PAHs 被认为是基因毒性致癌物,有致畸和致突变作用[1],而且由于其物理化学性质稳定,在自然环境中难以降解,是自然环境中持久性有机污染物的主要代表,受到国际上科学界的广泛关注。
迄今为止已发现有200多种PAHs,国际癌症研究中心(IARC)在二十世纪七十年代列出了94种具有致癌作用的化合物,这里面有15种是多环芳烃。多环芳烃能以气态或者颗粒态存在于大气、水、植物、土壤中。大气中PAHs以气、固两种形式存在,其中相对分子质量小的PAHs主要以气态形式存在,例如:芴、荧蒽、菲、芘等,大相对分子质量PAHs则绝大部分以颗粒态形式存在,例如:苯并芘、晕苯等。地表水体中的PAHs主要来源于大气沉降、地表径流、土壤淋溶、工业排放和城市废水排放等,已知地表水体中的多环芳烃有20余种,它们通过吸附在悬浮性固体上、溶解于水和呈乳化状态这3种方式存在于水体中[2]。PAHs对土壤的污染也极其严重,它们最初的形态大多数为气态,部分冷却后形成颗粒物或吸附在颗粒物上,随着颗粒物的飘动发散在环境各处,通过沉降和降水冲洗作用而污染土壤,植物在生长过程中会从中吸收、转移并富集PAHs,植物腐烂后,PAHs又回到土壤中。由于多环芳烃具有脂溶性特征,可以通过大气沉降作用经过地表植物的叶片吸收进入植物体内,或者可以通过农业生产中污水灌溉等方式进入土壤中由植物吸收,从而在植物体内迁移、代谢和积累,进而通过食物链进入人体,威胁人类的健康[3]。
基于PAHs 的遗传毒性和致突变性评估,美国环境保护署(The United States Environmental Protection Agency,USEPA)及国际癌症研究机构(International Agency for Research on Cancer,IARC)将其中16种列为优先控制污染物[4]。《化学品注册、评估、许可和限制法规》(REACH)附件管控PAHs 8项(包括:Bap、Bep、BaA、CHR、BbFA、BjFA、BkFA、DBAhA),本研究将16种优先控制污染物与REACH附件管控8种多环芳烃结合,选择18种多环芳烃为检测指标。目前,已有一些研究关注到中药材中的多环芳烃残留问题[5-6],但未根据中药不同部位的特点针对性地建立前处理方法,且未按中药的服用特点进行风险评估,本研究针对种子果实类中药建立提取净化方法,建立18种多环芳烃的气相色谱质谱联用(GC-MS/MS)检测方法,对种子果实类中药进行多环芳烃残留筛查,并对种子果实类中药的多环芳烃残留量进行初步风险评估,用以评价种子果实类中药材多环芳烃残留的安全性。
1 仪器与试药
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GCMS-TQ8030型三重四级杆气质联用仪,配AOC0-20i自动进样器(日本岛津公司);AG135型电子分析天平(瑞士Mettler Toledo公司);Z206A型离心机(德国Hermle公司);Heid-vdvantage ML型旋转蒸发仪(德国Heidolph公司);KQ-300TDV型超声提取仪(中国昆山市超声仪器有限公司)。
18种多环芳烃对照溶液(PAH-mix25,批号:20829AB,质量浓度2 000 ng·μL-1),内标物为16种氘代多环芳烃同位素对照溶液(PAH-MIX 9 deuterated,批号:21205CY,质量浓度100 ng·μL-1,德国Dr. Ehrensorfer公司);正己烷和二氯甲烷为农残级(美国Fisher公司);分子印迹固相萃取小柱(上海安谱科学仪器有限公司,500 mg,6 mL)。18种多环芳烃信息见表1(其中,除去13、14号峰则为美国环保署优先控制的16种多环芳烃)。药材(市售)。
2 方法与结果
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2.1 色谱条件
色谱柱:毛细管色谱柱(0.25 mm×30 m,0.25 μm)DM-17ms;进样体积为1 μL,不分流进样;载气为高纯氦气,柱流速为1.5 mL·min-1;升温程序条件:起始温度80 ℃,保持0.5 min,以25 ℃·min-1升温至130 ℃,再以10 ℃·min-1升温至200 ℃,保持2 min,再以20 ℃·min-1升温至260 ℃,再以3 ℃·min-1升温至290 ℃,保持8 min,再以20 ℃·min-1升温至320 ℃,保持3 min。进样口温度为290 ℃;接口温度为280 ℃。
2.2 质谱条件
离子源:电子轰击(EI)源;电离能量70 eV;离子源温度为220 ℃;进样量1 μL,高压进样,进样时间0.5 min,溶剂延迟:4.0 min,多反应检测模式(MRM)。18种多环芳烃及相应同位素内标物保留时间及定量、定性离子见表2(18种多环芳烃中bep及bjf没有同位素内标,bep以bap-d12为同位素内标,bjf以bkf-d12为同位素内标)。
2.3 溶液制备
2.3.1 同位素内标溶液
精密量取16种氘代多环芳烃同位素对照溶液1 mL,加环己烷稀释至20 mL,作为同位素内标储备溶液(5 μg·mL-1)。使用时吸取储备液200 μL,用乙腈稀释至200 mL,作为同位素内标溶液(5 ng·mL-1)。
2.3.2 对照品溶液的制备
精密量取18种多环芳烃对照溶液1 mL置20 mL量瓶中,加同位素内标溶液稀释并定容至刻度,作为对照品储备溶液(2.5 μg·mL-1)。再将对照品储备溶液用同位素内标溶液(5 ng·mL-1)逐级稀释成多环芳烃质量浓度分别为2、5、10、20、50、100 ng·mL-1的系列混合对照溶液(同位素内标浓度均为5 ng·mL-1)。
2.3.3 供试品溶液的制备
取药材细粉1 g,精密加同位素内标溶液(5 ng·mL-1)1 mL,加正己烷30 mL,匀浆提取3 min,提取2次,合并提取液,减压浓缩至5 mL,过MIP-PAH固相萃取小柱(用5 mL二氯甲烷活化固相萃取小柱,重复3次后用5 mL正己烷平衡),用10 mL正己烷淋洗后用10 mL二氯甲烷分2次洗脱,收集流出的二氯甲烷洗脱液,收集洗脱液,洗脱液用氮气吹干后用1 mL正己烷复溶,进行 GC-MS/MS 分析。
2.4 方法学考察
2.4.1 线性关系
将多环芳烃质量浓度分别为2、5、10、20、50 ng·mL-1的系列混合标准溶液(内标物质量浓度均为5 ng·mL-1)进样,测定。以18种多环芳烃及其对应同位素内标的浓度比值为横坐标X,以18种多环芳烃及其对应同位素内标的定量离子的峰面积为纵坐标Y,绘制标准工作曲线。18种多环芳烃在一定的浓度范围内有较好的线性关系,r均大于0.999,见表3。
2.4.2 精密度
分别精密吸取多环芳烃对照溶液(浓度为5 ng·mL-1),重复进样6次,计算峰面积平均值及相对标准偏差(RSD),RSD均小于10%,结果表明,精密度良好。
2.4.3 灵敏度
将对照品稀释至信噪比(S/N=10),以该浓度按供试品溶液制备方法折算出待测物中的浓度,作为本方法定量限。结果表明,各成分定量限在0.2~1 μg·kg-1之间,可满足分析方法要求。结果见表3。
2.4.4 重复性
精密称取样品1 g(木瓜),按供试品溶液制备方法分别平行制备6份,测定,计算,结果见表4。结果表明,检测的6种多环芳烃RSD均小于10%,可满足方法学要求。
2.4.5 回收率
称取木瓜(样品2)1 g,加多环芳烃对照溶液1 mL(浓度分别2,5,50 ng·mL-1),平行制备3份,加正己烷30 mL,匀浆提取3 min,提取2次,合并提取液,减压浓缩至5 mL,过MIP-PAH固相萃取小柱(用5 mL二氯甲烷活化固相萃取小柱,重复3次后用5 mL正己烷平衡),用10 mL正己烷淋洗后用10 mL二氯甲烷分2次洗脱,收集流出的二氯甲烷洗脱液,洗脱液用氮气吹干后用1 mL正己烷复溶,进行GC-MS/MS分析,见表5。
3 样品测定结果
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本研究合计测定了15个品种42批次的种子果实类中药材样品,测定结果显示种子果实类中药中存在18种多环芳烃残留量,PAHs的含量汇总和检出率见表6。
从汇总结果看,PAH单体浓度范围为未检出(no detected, ND)-2 492 μg·kg-1,其中,苯并(j)荧蒽的检出量最大,18种PAHs之和质量浓度范围为117.5~11 553.0 μg·kg-1, 轻质多环芳烃的质量浓度范围为50~5 061 μg·kg-1,重质多环芳烃的质量浓度范围为ND~4 333 μg·kg-1。从污染多环芳烃的环数来说,多环芳烃污染是以2、3和4环的轻质PAHs为主,平均占18种PAHs之和的77%,而5 环和6环的重质PAHs所占比重较低。从检出率来看,萘、芴、菲、蒽、荧蒽、芘、苯并(a)蒽的检出率均超90%。检测的42批次种子果实类中药材样品中,二苯并(a,h)蒽和苯并(ghi)苝的检出率较低,均低于50%,典型致癌物质苯并(a)芘检出率达到65%。
各个种子果实类样品中18种多环芳烃的平均浓度见表7。本文对苯并(a)芘、PAH2、PAH4和PAH8作为中药材中PAHs污染及其健康影响的指示物进行统计,分别统计了它们的检出范围及检出率,检测分析结果见表6。苯并(a)芘、PAH2、PAH4和PAH8检出范围为ND-44 μg·kg-1,ND-300 μg·kg-1、0.3~615 μg·kg-1、0.4~1 866 μg·kg-1,平均检出值分别为4.6、31.3、62.5、121.0 μg·kg-1。
从具体品种看,炒山楂、栀子、乌梅炭三个品种的PAH4均值超过100 μg·kg-1, 炒山楂、栀子、乌梅炭、山萸肉4个品种的苯并(a)芘均值超过5 μg·kg-1,玉竹、郁金两个品种的PAH2均值超过50 μg·kg-1,炒山楂、栀子、乌梅炭、陈皮4个品种的PAH8均值超过100 μg·kg-1,这些品种的PAHs的污染较为严重。本研究收集的样品涉及药材及相应饮片,麦芽和炒麦芽、山楂和炒山楂、乌梅和乌梅炭、炒白扁豆和白扁豆,从测定结果比对看,麦芽和炒麦芽、炒白扁豆和白扁豆多环芳烃的检测数值未见明显差异,而从山楂和炒山楂、乌梅和乌梅炭2种药对检测结果比较,则多环芳烃的量明显增加,说明炮制后多环芳烃有增加的趋势,可能和品种及炮制方法相关,值得进一步研究。
4 初步风险评估
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4.1 毒性当量因子(TEF)估算
本研究选用毒性当量因子(toxic equivalency factor,TEF)法估算16种优控PAHs相对苯并(a)芘(BaP)的总毒性当量浓度。在所有多环芳烃中,BaP具有最高的致癌性,因此多环芳烃的致突变性以BaP当量(BaPeq)表示。毒性当量因子法是由世界卫生组织(WHO)建立的,是一种基于剂量相加对多种物质暴露风险的综合评价方法,是将混合物中的每种成分与指示化合物的毒性相比来计算其当量。该方法以BaP为标准参照物,其毒性当量因子(TEF)值设定为1,将其他PAHs与等量的BaP进行毒性大小比较,得出各个PAHs的TEF值。现在大多采用Nisbet[7]提出的各个多环芳烃相对于BaP的TEF值,各个PAHs对BaP的TEF值见表1。通过公式1计算16种优控PAHs相对苯并(a)芘(BaP)的毒性当量浓度TEQBap。
$ \mathrm{TEQ}_{\text {Bap }}=\sum_{i=1}^{n} \mathrm{BaP}_{\text {eqi }}=\sum_{i=1}^{n} \mathrm{BaP}_{\text {eqi }} \rho_{\mathrm{i}} \times \mathrm{TEF}_{i}$
式中:ρi为第i个PAHs的质量浓度(μg·kg-1);TEQBap为相对BaP的总毒性当量浓度;TEFi为第i个PAHs对应的TEF值。
4.2 致癌风险评价
多环芳烃属于致癌物质,评估多环芳烃的增加终生癌症风险采用“个人因接触潜在致癌物(如多环芳烃)而终生罹患癌症的增加概率[8]的方法。增加终生致癌风险(Incremental lifetime cancer risk,ILCR)是指人暴露于某种可能致癌物时,可能增加的患癌风险。ILCR是指个体在一生中因暴露于潜在致癌物而发生癌症的概率增量,可通过公式2进行估算。
ILCR=TEQBap×DR×EF×SF×CF×ED/(BW×AT)
式中:ILCR为PAHs在某剂量下可致人群终生致癌风险;TEQBap为PAHs相对于BaP的等效致癌毒性(μg·kg-1),以公式1进行计算;DR为中药材的摄入量(g·d-1),以20 g·d-1计;EF为暴露频率,每年90 d[9];SF为BaP的致癌风险系数经口暴露数值,7.3 kg·d·mg-1[10];ED为暴露年数(a);BW为人均体质量以60 kg计;AT为人群的预期寿命(a);CF为转化因子10-6 kg·mg-1。选用USEPA 推荐的参数值:ED 对于非致癌物取30a,对于致癌物取70a;AT对非致癌物取30a(10 950 d),对于致癌物取70a(25 550 d)[11-13]。
依据US EPA对ILCR的潜在致癌风险区间,当ILCR≤10-6时表示不存在致癌风险或其致癌风险可以忽略,不需采取进一步的措施;当ILCR>10-4时表示具有较大的致癌风险,已经超过可承受的癌症风险水平上限,风险是不可接受的,必须要采取相应的行动;当 ILCR介于二者之间时,则表示存在低致癌风险或潜在致癌风险,但还未达到优先级风险水平[11]。
4.3 结果分析
根据公式1计算得到不同种类种子果实类中药材中16种优控PAHs相对BaP的毒性当量浓度TEQBap,再根据公式2计算得到种子果实类中药材PAHs污染的潜在致癌风险评价结果(表8)。从评估结果可以看出,麦芽、炒麦芽、山楂、木瓜、山萸肉、诃子、薏苡仁、乌梅、白扁豆、炒白扁豆、罗汉果的ILCR值小于10-6,存在的风险较低,而炒山楂、陈皮、栀子、山萸肉、乌梅炭、桑葚、麸炒枳实的ILCR值介于10-4~10-6之间,表明可能存在潜在致癌风险,需要我们的关注。
5 讨论
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多环芳烃为脂溶性化合物,易溶于正己烷、丙酮、二氯甲烷等非极性或中等极性有机溶剂,因此提取溶剂常选择正己烷、丙酮或二氯甲烷等有机溶剂。本研究比较了乙腈和正己烷对 18种 PAHs的提取效果,结果显示乙腈和正己烷均能将中药材中的多环芳烃提取出来,提取效率无明显差别。考虑到后续试验操作无需溶剂转换,本实验以正己烷为提取溶剂。
多环芳烃具有刚性平面结构和多个共轭双键,且热稳定性强,所以在用质谱作为检测器时,能够得到大的分子离子峰和很少的碎片离子,因此有些多环芳烃只能找到一组监测离子。
多环芳烃常用的净化方法有中性氧化铝柱、HLB 小柱、分子印迹柱、 凝胶色谱净化(GPC)、QuEChERS 、C18固相萃取等净化技术[14-16],本文考察了几种净化方法对种子果实类样品的净化效果,考虑净化效果、实验成本等综合因素, 我们选择分子印迹技术对种子果实类样品进行净化提取。
多环芳烃的风险评估方法有MOE(暴露边界值)[17]方法,HI(危害指数)法[18]及TEF (毒性当量因子)法[5],其中MOE及HI法仅能对其中几种多环芳烃的风险进行评估,不能全面反应多种多环芳烃的风险,而TEF法综合考虑了各种多环芳烃的风险。
基金
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  • 中国食品药品检定研究院关键技术研究基金项目资助(GTTS-2022-7-2)
文献
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2024年第59卷第8期
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  • 接收时间：2023-03-03
  • 首发时间：2026-04-08
  • 出版时间：2024-04-22
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  • 收稿日期：2023-03-03
基金
中国食品药品检定研究院关键技术研究基金项目资助(GTTS-2022-7-2)
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    中国食品药品检定研究院, 北京 102629

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*昝珂,男,副研究员 研究方向:中药、天然药质量控制及内源性有害物质研究 Tel:(010)53852092;
金红宇,男,主任药师 研究方向:中药、天然药质量控制及有害残留物分析 Tel:(010)53852076
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https://castjournals.cast.org.cn/joweb/zgyxzz/CN/1248601954910359570
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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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