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Article(id=1151881496383550239, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1151881493552394994, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20250121003, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1737388800000, receivedDateStr=2025-01-21, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1752559549660, onlineDateStr=2025-07-15, pubDate=1748102400000, pubDateStr=2025-05-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1752559549660, onlineIssueDateStr=2025-07-15, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1752559549660, creator=13701087609, updateTime=1752559549660, updator=13701087609, issue=Issue{id=1151881493552394994, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='10', pageStart='1', pageEnd='324', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1752559548986, creator=13701087609, updateTime=1756202008453, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1167159075906265916, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1151881493552394994, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1167159075906265917, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1151881493552394994, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=89, endPage=96, ext={EN=ArticleExt(id=1151923893209494156, articleId=1151881496383550239, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Analysis and risk assessment of 3-chloropropanol ester, glycidyl ester and phthalate ester content in Camellia oleifera seed oil of Jiangxi Province, columnId=1151923892655846010, journalTitle=Journal of Food Safety & Quality, columnName=Special Topic: Food Safety Risk Assessment and Risk Monitoring, runingTitle=null, highlight=null, articleAbstract=

Objective To understand the pollution situation of new risk factors such as 3-chloropropanol ester (3-MCPDE), glycidyl ester (GE), dibutyl phthalate (DBP) and bis(2-ethylhexyl) phthalate (DEHP) in Camellia oleifera seed oil of Jiangxi Province, and make risk assessment. Methods The content of 3-MCPDE, GE, DBP and DEHP in 29 batches of Camellia oleifera seed oil were determined by gas chromatography-mass spectrometry, and the exposure risk was analyzed by dietary exposure assessment method. Results The content of 3-MCPDE in Camellia oleifera seed oil ranged from 0.11 mg/kg to 4.52 mg/kg, the detection rate was 75.86%, and the problem rate was 10.34%. GE content ranged from 0.13 mg/kg to 11.76 mg/kg, the detection rate was 72.41%, and the problem rate was 44.83%. The content of DBP ranged from 0.43 mg/kg to 12.90 mg/kg, and the problem rate was 34.48%. The range of DEHP content was 0.57-9.69 mg/kg, the detection rate was 55.17%, and the problem rate was 20.69%. The average exposure of residents to DBP, DEHP, 3-MCPDE and GE through edible oil tea seed oil ranged from 0.56 μg/(kg·BW) to 0.75 μg/(kg·BW), and the exposure risk of DBP, DEHP and 3-MCPDE ranged from 1.12% to 37.37%. The exposure risk of margin of exposure (MOE) of GE was 3948.94 for men and 3347.52 for women, with both MOE values being below 10000. Conclusion Camellia oleifera seed oil poses a certain risk of contamination with 3-MCPDE, GE, DBP and DEHP. The likelihood of human health hazards from DBP, DEHP, and 3-MCPDE intake through Camellia seed oil is very low for residents. However, greater attention shall be paid to the health risks associated with GE exposure.

, correspAuthors=Wei-Ling CHEN, 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=Wei-Ling CHEN, Han LIAO, Xian-Biao LIU, Xiu-Ying ZENG, Zhi-Ming LI, Ming-Zhu ZHONG), CN=ArticleExt(id=1151923897336689378, articleId=1151881496383550239, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=江西省市售油茶籽油中3-氯丙醇酯、缩水甘油酯和邻苯二甲酸酯含量分析及其风险评估, columnId=1151923892995109553, journalTitle=食品安全质量检测学报, columnName=专题：食品安全风险评估与风险监测, runingTitle=null, highlight=null, articleAbstract=

目的 了解江西省市售油茶籽油中3-氯丙醇酯(3-chloropropanol ester, 3-MCPDE)、缩水甘油酯(glycidyl ester, GE)、邻苯二甲酸二正丁酯(dibutyl phthalate, DBP)及邻苯二甲酸二(2-乙基)己酯[bis(2-ethylhexyl) phthalate, DEHP]新型风险因子污染情况, 并对其进行风险评估。方法 采用气相色谱-质谱联用仪测定29批次油茶籽油中3-MCPDE、GE、DBP及DEHP含量, 并采用膳食暴露评估方法对其暴露风险进行分析。结果 油茶籽油中3-MCPDE含量范围为0.11~4.52 mg/kg, 检出率为75.86%, 问题率为10.34%; GE含量范围为0.13~11.76 mg/kg, 检出率为72.41%, 问题率为44.83%; DBP含量范围为0.43~12.90 mg/kg, 问题率为34.48%; DEHP含量范围为0.57~9.69 mg/kg, 检出率为55.17%, 问题率为20.69%。居民通过食用油茶籽油摄入DBP、DEHP、3-MCPDE和GE的平均暴露量范围为0.56~0.75 μg/(kg· BW), DBP、DEHP及3-MCPDE暴露风险范围为1.12%~37.37%, GE暴露风险的暴露边界(margin of exposure, MOE)值男性为3948.94, 女性为3347.52, MOE值均小于10000。结论 油茶籽油存在一定程度的3-MCPDE、GE、DBP及DEHP污染风险, 居民通过油茶籽油摄入DBP、DEHP及3-MCPDE对人体造成危害的可能性很小, 但对于GE暴露的健康风险需要更多的关注。

, correspAuthors=陈玮玲, authorNote=null, correspAuthorsNote=
* 陈玮玲(1992—), 女, 工程师, 主要研究方向为食品质量与安全。E-mail:
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Food Science, 2012, 33(20): 184-188., articleTitle=Simultaneous determination of 8 kinds of phthalic acid esters in plastic food packaging materials by high performance liquid chromatography, refAbstract=null)], funds=[Fund(id=1167158782380487331, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496383550239, awardId=GSJK202309, language=CN, fundingSource=江西省市场监督管理局科技项目(GSJK202309), fundOrder=null, country=null), Fund(id=1167158782443401892, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496383550239, awardId=20233BBF64002, language=CN, fundingSource=江西省重点研发计划项目(20233BBF64002), fundOrder=null, country=null), Fund(id=1167158782493733541, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496383550239, awardId=2023MK073, language=CN, fundingSource=国家市场监督管理总局科技计划项目(2023MK073), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1167158779494806122, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496383550239, xref=null, ext=[AuthorCompanyExt(id=1167158779499000427, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496383550239, companyId=1167158779494806122, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Ganzhou General Inspection and Testing Institute, Ganzhou 341000, China), AuthorCompanyExt(id=1167158779507389036, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496383550239, companyId=1167158779494806122, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=赣州市综合检验检测院, 赣州 341000)])], figs=[ArticleFig(id=1167158781583569559, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496383550239, language=EN, label=Fig.1, caption=Extraction ion chromatograms of 3-MCPDE and GE and their internal standard derivatives in Camellia oleifera seed oil, figureFileSmall=RydSIjMHYUgVTAeyvyId8w==, figureFileBig=zAWNzkZkFBpduHJfTA5rfA==, tableContent=null), ArticleFig(id=1167158781629706904, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496383550239, language=CN, label=图1, caption=油茶籽油中3-MCPDE和GE及其内标衍生物的提取离子色谱图

注: 3-MCPDE的保留时间=7.385 min; 13C3-3-MCPDE的保留时间=7.384 min; 3-MBPD的保留时间=7.740 min; 13C3-3-MBPD的保留时间=7.739 min; D5-3-MBPD的保留时间=7.723 min。

, figureFileSmall=RydSIjMHYUgVTAeyvyId8w==, figureFileBig=zAWNzkZkFBpduHJfTA5rfA==, tableContent=null), ArticleFig(id=1167158781688427161, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496383550239, language=EN, label=Table 1, caption=

Recoveries and precisions of 3-MCPDE and GE (n=6)

, figureFileSmall=null, figureFileBig=null, tableContent=
加标水平/ng 3-MCPDE
(以3-氯丙醇计)		 GE
(以缩水甘油计)
平均
回收率/%		 相对标准偏差/% 平均
回收率/%		 相对标准偏差/%
10 83.81 3.02 95.49 4.03
20 92.39 7.63 89.42 5.44
100 98.93 2.19 94.75 3.89
), ArticleFig(id=1167158781738758810, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496383550239, language=CN, label=表1, caption=

3-MCPDE和GE的回收率与精密度(n=6)

, figureFileSmall=null, figureFileBig=null, tableContent=
加标水平/ng 3-MCPDE
(以3-氯丙醇计)		 GE
(以缩水甘油计)
平均
回收率/%		 相对标准偏差/% 平均
回收率/%		 相对标准偏差/%
10 83.81 3.02 95.49 4.03
20 92.39 7.63 89.42 5.44
100 98.93 2.19 94.75 3.89
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Determination results of 3-MCPDE and GE in FAPAS vegetable oil quality control samples (mg/kg)

, figureFileSmall=null, figureFileBig=null, tableContent=
质控样 3-MCPDE
(以3-氯丙醇计)		 GE
(以缩水甘油计)
特性值 0.22 0.30
实测值 0.20 0.22
特性值区间 0.13~0.30 0.19~0.41
), ArticleFig(id=1167158781872976540, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496383550239, language=CN, label=表2, caption=

FAPAS植物油质控样品中3-MCPDE和GE测定结果(mg/kg)

, figureFileSmall=null, figureFileBig=null, tableContent=
质控样 3-MCPDE
(以3-氯丙醇计)		 GE
(以缩水甘油计)
特性值 0.22 0.30
实测值 0.20 0.22
特性值区间 0.13~0.30 0.19~0.41
), ArticleFig(id=1167158781927502493, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496383550239, language=EN, label=Table 3, caption=

Content of DBP, DEHP, 3-MCPDE and GE in different Camellia oleifera seed oil samples

, figureFileSmall=null, figureFileBig=null, tableContent=
样品 等级 含量/(mg/kg)
DBP DEHP 3-MCPDE(以3-MCPD计) GE(以缩水甘油计)
样品1 水酶法特级 12.90±0.34 4.71±0.09 ND 0.13±0.03
样品2 水酶法特级 9.04±0.42 9.69±0.24 ND ND
样品3 水酶法特级 0.66±0.16 4.81±0.30 ND ND
样品4 超临界CO₂萃取一级 ND 1.97±0.12 ND ND
样品5 鲜籽初榨特级 0.46±0.04 0.75±0.06 ND ND
样品6 压榨一级 0.43±0.02 ND 1.35±0.27 2.67±0.40
样品7 压榨一级 12.17±0.14 ND 1.85±0.07 11.76±0.35
样品8 压榨一级 1.06±0.04 ND 0.29±0.05 0.17±0.06
样品9 压榨一级 3.77±0.07 ND 0.34±0.05 0.17±0.03
样品10 压榨一级 ND 0.91±0.04 4.52±0.14 1.69±0.34
样品11 压榨一级 ND 0.58±0.03 2.41±0.30 3.60±0.41
样品12 压榨一级 1.39±0.39 ND 0.89±0.12 1.17±0.11
样品13 压榨一级 ND 1.30±0.03 2.40±0.16 1.39±0.07
样品14 压榨一级 1.49±0.04 1.02±0.06 0.16±0.05 0.20±0.01
样品15 压榨一级 ND 0.59±0.02 3.37±0.15 0.75±0.14
样品16 压榨一级 ND 0.57±0.05 2.66±0.20 0.50±0.20
样品17 压榨一级 ND 9.29±0.10 1.58±0.06 3.11±0.08
样品18 压榨一级 ND 1.37±0.04 ND ND
样品19 压榨一级 ND 1.30±0.08 ND ND
样品20 压榨一级 ND ND 1.28±0.12 1.41±0.28
样品21 压榨一级 ND ND 2.07±0.19 1.69±0.12
样品22 压榨一级 ND ND 0.30±0.03 ND
样品23 压榨一级 ND ND 0.51±0.02 0.74±0.03
样品24 压榨一级 ND ND 0.11±0.01 ND
样品25 浸出一级 ND 0.82±0.05 2.17±0.20 2.44±0.27
样品26 浸出一级 ND 9.44±0.12 1.66±0.19 2.92±0.40
样品27 压榨一级 ND ND 1.34±0.16 0.77±0.13
样品28 压榨二级 ND ND 1.23±0.16 2.45±0.41
样品29 浸出一级 ND ND 2.32±0.16 2.09±0.60
), ArticleFig(id=1167158781998805662, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496383550239, language=CN, label=表3, caption=

不同油茶籽油样品中DBP、DEHP、3-MCPDE和GE的含量

, figureFileSmall=null, figureFileBig=null, tableContent=
样品 等级 含量/(mg/kg)
DBP DEHP 3-MCPDE(以3-MCPD计) GE(以缩水甘油计)
样品1 水酶法特级 12.90±0.34 4.71±0.09 ND 0.13±0.03
样品2 水酶法特级 9.04±0.42 9.69±0.24 ND ND
样品3 水酶法特级 0.66±0.16 4.81±0.30 ND ND
样品4 超临界CO₂萃取一级 ND 1.97±0.12 ND ND
样品5 鲜籽初榨特级 0.46±0.04 0.75±0.06 ND ND
样品6 压榨一级 0.43±0.02 ND 1.35±0.27 2.67±0.40
样品7 压榨一级 12.17±0.14 ND 1.85±0.07 11.76±0.35
样品8 压榨一级 1.06±0.04 ND 0.29±0.05 0.17±0.06
样品9 压榨一级 3.77±0.07 ND 0.34±0.05 0.17±0.03
样品10 压榨一级 ND 0.91±0.04 4.52±0.14 1.69±0.34
样品11 压榨一级 ND 0.58±0.03 2.41±0.30 3.60±0.41
样品12 压榨一级 1.39±0.39 ND 0.89±0.12 1.17±0.11
样品13 压榨一级 ND 1.30±0.03 2.40±0.16 1.39±0.07
样品14 压榨一级 1.49±0.04 1.02±0.06 0.16±0.05 0.20±0.01
样品15 压榨一级 ND 0.59±0.02 3.37±0.15 0.75±0.14
样品16 压榨一级 ND 0.57±0.05 2.66±0.20 0.50±0.20
样品17 压榨一级 ND 9.29±0.10 1.58±0.06 3.11±0.08
样品18 压榨一级 ND 1.37±0.04 ND ND
样品19 压榨一级 ND 1.30±0.08 ND ND
样品20 压榨一级 ND ND 1.28±0.12 1.41±0.28
样品21 压榨一级 ND ND 2.07±0.19 1.69±0.12
样品22 压榨一级 ND ND 0.30±0.03 ND
样品23 压榨一级 ND ND 0.51±0.02 0.74±0.03
样品24 压榨一级 ND ND 0.11±0.01 ND
样品25 浸出一级 ND 0.82±0.05 2.17±0.20 2.44±0.27
样品26 浸出一级 ND 9.44±0.12 1.66±0.19 2.92±0.40
样品27 压榨一级 ND ND 1.34±0.16 0.77±0.13
样品28 压榨二级 ND ND 1.23±0.16 2.45±0.41
样品29 浸出一级 ND ND 2.32±0.16 2.09±0.60
), ArticleFig(id=1167158782078497439, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496383550239, language=EN, label=Table 4, caption=

Determination of 3-MCPDE and GE in Camellia oleifera seed oil samples by different methods (mg/kg)

, figureFileSmall=null, figureFileBig=null, tableContent=
样品 3-MCPDE(以3-MCPD计) GE(以缩水甘油计)
本方法 GB 5009.191—2024b 本方法 GB 5009.191—2024b
样品7 1.85±0.07 1.59 11.76±0.35 12.42
样品15 3.37±0.15 3.01 0.75±0.14 0.76
样品17 1.58±0.06 1.45 3.11±0.08 3.22
样品23 0.51±0.02 0.48 0.74±0.03 0.72
样品26 1.66±0.19 1.46 2.92±0.40 3.29
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不同方法测定油茶籽油样品中3-MCPDE和GE的含量(mg/kg)

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样品 3-MCPDE(以3-MCPD计) GE(以缩水甘油计)
本方法 GB 5009.191—2024b 本方法 GB 5009.191—2024b
样品7 1.85±0.07 1.59 11.76±0.35 12.42
样品15 3.37±0.15 3.01 0.75±0.14 0.76
样品17 1.58±0.06 1.45 3.11±0.08 3.22
样品23 0.51±0.02 0.48 0.74±0.03 0.72
样品26 1.66±0.19 1.46 2.92±0.40 3.29
), ArticleFig(id=1167158782208520865, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496383550239, language=EN, label=Table 5, caption=

Dietary exposure situation of DBP, DEHP, 3-MCPDE and GE in Camellia oleifera seed oil

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目标物 中位值/(mg/kg) 男性 女性
EDI/[μg/(kg·BW)] 暴露风险/% EDI/[μg/(kg·BW)] 暴露风险/%
DBP 1.44 0.62 6.21 0.73 7.32
DEHP 1.30 0.56 1.12 0.66 1.32
3-MCPDE 1.47 0.63 31.68 0.75 37.37
GE 1.41 0.61 3948.94* 0.72 3347.52*
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油茶籽油中DBP、DEHP、3-MCPDE和GE的膳食暴露情况

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目标物 中位值/(mg/kg) 男性 女性
EDI/[μg/(kg·BW)] 暴露风险/% EDI/[μg/(kg·BW)] 暴露风险/%
DBP 1.44 0.62 6.21 0.73 7.32
DEHP 1.30 0.56 1.12 0.66 1.32
3-MCPDE 1.47 0.63 31.68 0.75 37.37
GE 1.41 0.61 3948.94* 0.72 3347.52*
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江西省市售油茶籽油中3-氯丙醇酯、缩水甘油酯和邻苯二甲酸酯含量分析及其风险评估
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陈玮玲 * , 廖涵 , 刘贤标 , 曾秀英 , 李枝明 , 钟明珠
食品安全质量检测学报 | 专题：食品安全风险评估与风险监测 2025,16(10): 89-96
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食品安全质量检测学报 | 专题：食品安全风险评估与风险监测 2025, 16(10): 89-96
江西省市售油茶籽油中3-氯丙醇酯、缩水甘油酯和邻苯二甲酸酯含量分析及其风险评估
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陈玮玲* , 廖涵, 刘贤标, 曾秀英, 李枝明, 钟明珠
作者信息
  • 赣州市综合检验检测院, 赣州 341000

通讯作者:

* 陈玮玲(1992—), 女, 工程师, 主要研究方向为食品质量与安全。E-mail:
Analysis and risk assessment of 3-chloropropanol ester, glycidyl ester and phthalate ester content in Camellia oleifera seed oil of Jiangxi Province
Wei-Ling CHEN* , Han LIAO, Xian-Biao LIU, Xiu-Ying ZENG, Zhi-Ming LI, Ming-Zhu ZHONG
Affiliations
  • Ganzhou General Inspection and Testing Institute, Ganzhou 341000, China
出版时间: 2025-05-25 doi: 10.19812/j.cnki.jfsq11-5956/ts.20250121003
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摘要
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目的 了解江西省市售油茶籽油中3-氯丙醇酯(3-chloropropanol ester, 3-MCPDE)、缩水甘油酯(glycidyl ester, GE)、邻苯二甲酸二正丁酯(dibutyl phthalate, DBP)及邻苯二甲酸二(2-乙基)己酯[bis(2-ethylhexyl) phthalate, DEHP]新型风险因子污染情况, 并对其进行风险评估。方法 采用气相色谱-质谱联用仪测定29批次油茶籽油中3-MCPDE、GE、DBP及DEHP含量, 并采用膳食暴露评估方法对其暴露风险进行分析。结果 油茶籽油中3-MCPDE含量范围为0.11~4.52 mg/kg, 检出率为75.86%, 问题率为10.34%; GE含量范围为0.13~11.76 mg/kg, 检出率为72.41%, 问题率为44.83%; DBP含量范围为0.43~12.90 mg/kg, 问题率为34.48%; DEHP含量范围为0.57~9.69 mg/kg, 检出率为55.17%, 问题率为20.69%。居民通过食用油茶籽油摄入DBP、DEHP、3-MCPDE和GE的平均暴露量范围为0.56~0.75 μg/(kg· BW), DBP、DEHP及3-MCPDE暴露风险范围为1.12%~37.37%, GE暴露风险的暴露边界(margin of exposure, MOE)值男性为3948.94, 女性为3347.52, MOE值均小于10000。结论 油茶籽油存在一定程度的3-MCPDE、GE、DBP及DEHP污染风险, 居民通过油茶籽油摄入DBP、DEHP及3-MCPDE对人体造成危害的可能性很小, 但对于GE暴露的健康风险需要更多的关注。

油茶籽油  /  3-氯丙醇酯  /  缩水甘油酯  /  邻苯二甲酸二正丁酯  /  邻苯二甲酸二(2-乙基)己酯  /  膳食暴露评估

Objective To understand the pollution situation of new risk factors such as 3-chloropropanol ester (3-MCPDE), glycidyl ester (GE), dibutyl phthalate (DBP) and bis(2-ethylhexyl) phthalate (DEHP) in Camellia oleifera seed oil of Jiangxi Province, and make risk assessment. Methods The content of 3-MCPDE, GE, DBP and DEHP in 29 batches of Camellia oleifera seed oil were determined by gas chromatography-mass spectrometry, and the exposure risk was analyzed by dietary exposure assessment method. Results The content of 3-MCPDE in Camellia oleifera seed oil ranged from 0.11 mg/kg to 4.52 mg/kg, the detection rate was 75.86%, and the problem rate was 10.34%. GE content ranged from 0.13 mg/kg to 11.76 mg/kg, the detection rate was 72.41%, and the problem rate was 44.83%. The content of DBP ranged from 0.43 mg/kg to 12.90 mg/kg, and the problem rate was 34.48%. The range of DEHP content was 0.57-9.69 mg/kg, the detection rate was 55.17%, and the problem rate was 20.69%. The average exposure of residents to DBP, DEHP, 3-MCPDE and GE through edible oil tea seed oil ranged from 0.56 μg/(kg·BW) to 0.75 μg/(kg·BW), and the exposure risk of DBP, DEHP and 3-MCPDE ranged from 1.12% to 37.37%. The exposure risk of margin of exposure (MOE) of GE was 3948.94 for men and 3347.52 for women, with both MOE values being below 10000. Conclusion Camellia oleifera seed oil poses a certain risk of contamination with 3-MCPDE, GE, DBP and DEHP. The likelihood of human health hazards from DBP, DEHP, and 3-MCPDE intake through Camellia seed oil is very low for residents. However, greater attention shall be paid to the health risks associated with GE exposure.

Camellia oleifera seed oil  /  3-chloropropanol ester  /  glycidyl ester  /  dibutyl phthalate  /  bis(2-ethylhexyl) phthalate  /  dietary exposure assessment
陈玮玲, 廖涵, 刘贤标, 曾秀英, 李枝明, 钟明珠. 江西省市售油茶籽油中3-氯丙醇酯、缩水甘油酯和邻苯二甲酸酯含量分析及其风险评估. 食品安全质量检测学报, 2025 , 16 (10) : 89 -96 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250121003
Wei-Ling CHEN, Han LIAO, Xian-Biao LIU, Xiu-Ying ZENG, Zhi-Ming LI, Ming-Zhu ZHONG. Analysis and risk assessment of 3-chloropropanol ester, glycidyl ester and phthalate ester content in Camellia oleifera seed oil of Jiangxi Province[J]. Journal of Food Safety & Quality, 2025 , 16 (10) : 89 -96 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250121003
正文
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0 引言
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油茶籽油是从油茶树的果实中提取而来的天然保健木本植物油[1], 富含维生素E, 谷甾醇、角鲨烯、多酚等活性成分, 具有降血脂、护肝、抗炎、调节免疫力、治疗皮肤病等保健作用[2-3]。油茶籽油被誉为“东方橄榄油”, 被列入《本草纲目》中的药用油[4], 越来越受到国内外研究学者的广泛关注, 也越来越受到消费者的青睐, 是我国高端植物油的重要来源之一。
随着油茶产业的发展, 市场规模的扩大和消费量的增加, 油茶籽油的质量安全问题逐渐成为人们关注的焦点, 为行业的发展带来了新的机遇和挑战。此外, 油茶籽油在种植、加工和储存过程中可能会伴随产生危害人体健康的有害物质如3-氯丙醇酯(3-chloropropanol ester, 3-MCPDE)、缩水甘油酯(glycidyl ester, GE)、邻苯二甲酸酯(phthalate acid esters, PAEs)、多环芳烃、反式脂肪酸等[5-6], 其中, 3-MCPDE、GE和PAEs是近年来油茶籽油行业广泛关注的新型污染物。研究表明, 3-MCPDE、GE主要是在高温精炼脱臭阶段产生的副产物[7-8], 在人体内被水解为3-氯丙醇和缩水甘油, 具有生殖毒性、肾脏毒性、神经毒性、遗传毒性及潜在的致癌性[9-10], 同时3-氯丙醇被国际癌症研究机构列为2B级致癌物, 缩水甘油被列为2A级致癌物[11-12]。FAN等[13]研究发现杭州市市售241种植物油中3-MCPDE的平均含量为0.8 mg/kg, 其中茶油的平均含量最高, 检出率达100%, 橄榄油的平均含量最低, 检出率为41.2%。CUI等[14]研究发现来自不同省份的1343批次植物油样品中3-MCPDE的检出率高达78.7%, 其中茶油的检出率最高为87.8%。由此发现, 不同种类的植物油在污染物含量上存在显著差异, 油茶籽油可能更容易受到3-MCPDE的污染。目前, 人们从日常饮食中引入3-MCPDE和GE的基本来源主要来自精制植物油, 而精制植物油广泛应用于食品工业中, 因此, 3-MCPDE和GE作为精制植物油加工过程中产生的污染物, 已广泛存在于日常饮食中[15]。
PAEs是一种脂溶性物质, 主要来源于生产加工过程中塑料制品的污染[16-17], 很容易通过与塑料制品的接触迁移到油茶籽油中, 具有一定的生殖毒性、发育毒性及致癌性[18-19]。据报道, 市场流通的油茶籽油PAEs不符合要求主要体现在邻苯二甲酸二正丁酯(dibutyl phthalate, DBP)、邻苯二甲酸二(2-乙基)己酯[bis(2-ethylhexyl) phthalate, DEHP]两项指标上[20], 尤其是无精炼工艺的小作坊企业生产的油茶籽油产品。在油脂精炼过程中, 3-MCPDE和GE通常会一起存在, 且市面上大多数成品油茶籽油中检出率均较高, 说明3-MCPDE、GE和PAEs在油茶籽油中污染比较普遍。目前, 油茶籽油生产企业主要在精炼过程中通过高温、高压去除PAEs, 但同时容易产生3-MCPDE和GE。若降低温度, 可一定程度避免3-MCPDE和GE产生但无法去除PAEs, 两者很难达到平衡。经调研, 一方面油茶籽油经营主体关于3-MCPDE、GE和PAEs的风险防控意识较弱, 很少关注3-MCPDE、GE和PAEs的含量; 另一方面常态化监测这3项指标对经营主体而言成本太高, 国家尚无健全的限量标准, 如果不加强监管, 将对人体健康产生巨大的潜在危害[21]。目前, 油茶籽油在活性成分、掺伪鉴别和常规品质分析如酸值、过氧化值、碘值、皂化值、脂肪酸组成等方面相对报道较多, 而活性成分的形态组成、结构鉴定、指纹图谱及污染物方面缺乏系统性的研究。
本研究通过测定市售油茶籽油中潜在风险因子DBP、DEHP、3-MCPDE和GE指标, 对油茶籽油进行风险评估, 是对现行油茶籽油标准中有害成分指标的进一步补充, 为将来标准的制定提供依据, 为油茶籽油的质量安全监测和控制提供参考, 助力油茶产业高质量发展。
1 材料与方法
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1.1 材料与试剂
29批次油茶籽油样品均为江西省内市售, 于2023—2024年随机采集于江西省内流通市场。样品为采用压榨、浸出、水酶法、超临界CO2萃取等工艺的精炼成品油。
3-氯-1,2-丙二醇棕榈酸二酯(CAS: 51930-97-3, 纯度≥98%)、13C3-3-氯-1,2-丙二醇棕榈酸二酯(13C3-3-chloro-1,2- propylene glycol palmitate diester, 13C3-3-MCPDE, 纯度≥96%)、缩水甘油棕榈酸酯(CAS: 7501-44-2, 纯度≥98%)、D5-缩水甘油棕榈酸酯(CAS: 1794941-80-2, D5-glycidyl palmitate, D5-GE, 纯度≥98%)、16种邻苯二甲酸酯类混合液体标准品(质量浓度1000 μg/mL)(天津阿尔塔科技有限公司); 乙腈、甲醇、正己烷、甲苯、丙酮(色谱纯, 美国赛默飞世尔科技有限公司); 叔丁基甲醚(色谱纯)、苯基硼酸(纯度≥97%)、溴化钠(纯度≥99.5%)(上海麦克林生化科技有限公司); 氢氧化钠、无水硫酸钠、硫酸、乙二醇(分析纯, 西陇科学股份有限公司)。
1.2 仪器与设备
TRACE 1300-ISQ 7000气相色谱质谱联用仪(美国赛默飞世尔科技有限公司); 8890-7000 D全自动顶空-气相色谱质谱联用仪、DB-5 MS色谱柱(30 m×0.25 mm, 0.25 μm)(美国安捷伦科技有限公司); PSA/Silica复合填料玻璃柱(1000 mg, 6 mL, 天津博纳艾杰尔科技有限公司)。
1.3 3-MCPDE和GE的检测
参照GB 5009.191—2024《食品安全国家标准 食品中氯丙醇及其脂肪酸酯、缩水甘油酯的测定》方法, 结合文献[22]所述, 称取0.1 g试样于4 mL玻璃溶剂瓶中, 准确加入100 μL混合内标工作液, 混匀后加入100 μL甲苯和200 μL甲基叔丁基醚, 混匀后于10 ℃±1 ℃下冷却6 min, 之后加入200 μL在10 ℃下预先冷却2 h的0.35 mol/L氢氧化钠-甲醇溶液, 立即涡旋后于10 ℃±1 ℃下放置7 min, 然后加入600 μL酸化溴化钠溶液(600 g/L), 涡旋。在上述水解液中加入600 μL异辛烷, 涡旋进行液-液萃取, 静置分层后弃去异辛烷层, 重复两次。下层水溶液中加入100 μL苯基硼酸溶液, 涡旋后加入1.0 mL异辛烷, 弃去下层, 然后加入100 μL 1%乙二醇溶液, 涡旋, 静置分层, 取上层溶液经无水硫酸钠脱水后过膜待上机。
测得3-MCPDE、GE及内标衍生物的峰面积, 由峰面积比值通过相应标准曲线计算得到3-MCPDE和GE的质量, 试样中3-MCPDE和GE总量的含量按公式(1)计算:
$X=\frac{M_{1}}{m} \times \frac{1000}{1000}$
式中: X为样品中3-MCPDE和GE总量的含量(以氯丙醇和缩水甘油计), μg/kg; M1为标准曲线计算的中3-MCPDE和GE的质量, ng; m为试样的质量, g; 1000为换算系数。
在3-MCPDE标准系列中, 以3-MCPDE与13C3-3-MCPDE的峰面积比为横坐标, 3-溴-1,2-丙二醇(3-bromo-1,2-propanediol, 3-MBPD)与13C3-3-MBPD的峰面积比为纵坐标, 得到线性方程。3-MCPDE转化而成3-MBPD峰面积的按公式(2)计算:
$A_{1}=\left(\frac{A_{2}}{A_{\mathrm{IS} 2}} \times a+b\right) \times A_{\mathrm{IS} 1}$
式中: A1为试样中由3-MCPDE转化而成3-MBPD的峰面积; A2为试样中3-MCPDE的峰面积; AIS2为试样中内标13C3-3-MCPDE的峰面积; a为回归方程的斜率; b为回归方程的截距; AIS1为试样中由内标13C3-3-MCPDE转化而成13C3-3-MBPD的峰面积。
根据GE的标准曲线, 由试样峰面积比值计算得到GE的总量, 并由公式(2)中计算3-MCPDE转化得到3-MBPD(以缩水甘油计)的质量, 即M转, 扣除3-MCPDE转化得到3-MBPD的量, 得到试样中GE的含量按公式(3)计算:
$G_{1}=G_{\text {总 }}-\frac{M_{\text {线 }}}{m} \times \frac{1000}{1000}$
式中: G1为试样中GE的含量, μg/kg; G总为GE的总量, μg/kg; M转为通过GE的标准曲线计算3-MCPDE转化得到3-MBPD的质量, ng; m为试样的质量, g; 1000为换算系数。
1.4 DBP和DEHP的检测
参照GB 5009.271—2016《食品安全国家标准 食品中邻苯二甲酸酯的测定》方法, 准确称取油茶籽油0.5 g于20 mL玻璃顶空瓶中, 加入2 mL正己烷饱和的乙腈溶液, 涡旋充分混匀后超声提取20 min, 然后4000 r/min离心5 min, 上清液转移至另一个20 mL玻璃顶空瓶中, 残渣再次用2 mL正己烷饱和的乙腈提取2次, 合并3次上清液经SPE净化后于40 ℃氮吹至近干, 用2 mL正己烷定容待上机。
1.5 暴露评估方法
采用膳食暴露评估方法对油茶籽油中3-MCPDE、GE、DBP和DEHP的污染水平进行评价[23-25]。按照3-MCPDE、GE、DBP和DEHP监测结果的中位数评估相应的暴露情况。按公式(4)计算:
EDIaverage=Caverage×Faverage/BW
式中: EDIaverage为每日平均暴露量(estimated daily intake), [μg/(kg·BW)]; Caverage为油茶籽油中污染物含量, mg/kg; Faverage为每日食用植物油摄入量, 以g/d; BW为人群平均体质量, kg。
3-MCPDE、DBP和DEHP暴露风险按公式(5)计算:
暴露风险/%=(EDI/TDI)×100%
式中: TDI为每日最大耐受摄入量(tolerable daily intake, TDI), μg/(kg·BW); 以植物油中污染物的每日平均暴露量与每日最大耐受摄入量的比值评估暴露情况, 暴露风险与该值呈正相关以揭示是否有暴露风险, 其中3-MCPDE、DBP和DEHP的TDI分别为2.0 μg/(kg·BW)、0.01 mg/(kg·BW)、0.05 mg/(kg·BW)[26-27], 我国居民人均每日食用油的摄入量根据中国居民膳食指南推荐摄入量上限30 g计算, 根据《中国居民营养与慢性病状况报告(2020年)》数据, 中国居民成年男性和女性的平均体重分别为69.6 kg和59.0 kg。
由于未制定针对GE的TDI指导值, 本研究采用暴露边界(margin of exposure, MOE)值来评估GE的膳食暴露风险, 采用联合国粮农组织/世界卫生组织食品添加剂联合专家委员会制定的产生10%肿瘤发生率的基准剂量(benchmark dose, BMD)值的95%置信区间下限值(BMDL10)为2.4 mg/(kg· BW)来计算GE的MOE值, 当MOE<10000时, 表示存在一定的健康风险, 当MOE>10000时, 表示暴露风险处于可接受水平[28-29]。按公式(6)计算:
MOE=BMDL10×103/EDI
1.6 数据处理
采用Excel 2019进行数据处理, 并以平均值±标准偏差(n=3)的形式表示, Origin Pro 2022作为绘图工具。
2 结果与分析
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2.1 油茶籽油中3-MCPDE和GE的方法评价
本研究采用同位素稀释-碱水解同时测定两种化合物, 在水解过程中, 少部分3-MCPDE的水解产物可转化为缩水甘油, 溴化后生成与GE处理后的同一产物3-溴-1,2-丙二醇(3-bromopropane-1,2-diol, 3-MBPD)。因此, 在计算试样中GE含量时, 需要扣除由3-MCPDE水解转化的含量, 从而获得准确的结果。在空白基质中添加标准溶液, 定量离子色谱图见图1, 以3倍信噪比时的浓度为检出限, 3倍检出限为定量限, 在本研究条件下, 以样品质量为0.1 g计, 油茶籽油中3-MCPDE和GE的检出限和定量限分别为4 μg/kg和12 μg/kg。
为了保证分析结果的准确性, 在低含量油茶籽油样品中添加低、中、高3个加标水平进行加标, 结果见表1, 两种化合物的平均回收率为83.81%~98.93%, 相对标准偏差为2.19%~7.63%, 表明该方法重现性良好, 精密度良好, 符合分析要求。此外, 本研究采用FAPAS质控样品(T2679QC)进行数据准确性验证, 测定结果见表2, 两个项目的检测结果均在特性值范围内, 说明该方法准确可靠, 可应用于样品的检测分析。
2.2 油茶籽油中3-MCPDE和GE检测结果
3-MCPDE和GE主要是在油茶籽油精炼加工过程中产生的污染物, 研究表明, 食用油毛油经脱色、脱臭工艺后, 其含量随着温度的升高而显著增加, 同时如果脱色过程使用的脱色剂引入了氯离子也会导致3-MCPDE含量大幅升高。此外, 精炼食用油被广泛作为食品生产加工原材料应用于食品加工工业, 因此, 3-MCPDE和GE在食品中的污染情况亦非常的普遍。
目前, 国内尚无针对3-MCPDE和GE的限量标准, 仅在国家食品安全风险监测中规定油茶籽油中3-MCPDE和GE限量分别为2.50 mg/kg和1.0 mg/kg。本研究对29批次油茶籽油中的3-MCPDE和GE含量进行检测, 结果见表3, 其中有22批次样品检出3-MCPDE, 3批次样品超限量, 含量范围为0.11~4.52 mg/kg, 检出率为75.86%, 问题率为10.34%。此外, 有21批次样品检出GE, 13批次样品超限量, 含量范围为0.13~11.76 mg/kg, 检出率达72.41%, 问题率为44.83%。从生产工艺角度来看, 水酶法特级、超临界CO₂萃取一级、鲜籽初榨特级油茶籽油3-MCPDE和GE的检出率较低, 压榨一级和浸出一级油茶籽油检出率普遍偏高, 个别样品GE含量甚至超过限量值十几倍, 说明该类型生产工艺加工的油茶籽油污染问题亟需重视。研究表明, 油茶籽油的污染风险可能直接关联其质量等级和精炼度, 等级越低精炼度越高, 3-MCPDE和GE的污染风险也越高。本研究与国内具备中国计量认证(China metrology accreditation, CMA)资质的检验检测实验室针对GB 5009.191—2024(第一篇 第二法)进行了实验室间方法比对, 结果见表4, 从比对结果可以看出, 本实验室测定值与GB 5009.191—2024差异不显著, 在标准误差范围内, 说明该方法准确可靠。
2.3 油茶籽油中DBP和DEHP检测结果
油茶籽油中PAEs污染主要源于原料和生产过程塑料制品的接触, 原料的污染包括土壤污染、塑料制品的长时间接触或在塑料制品上晾晒油茶籽; 加工环节的污染包括使用或接触了塑料制品的管道、滤纸、垫片、包饼布、生料带、传送带等; 包装设备的污染, 如使用了不达标的塑料制品储存油茶籽油。此外, 研究表明, 在油脂精炼脱臭过程中, PAEs的含量随温度的升高而显著下降, 原因可能是高温会导致PAEs的分解[30]。
按照国家市场监督管理总局《关于食品中“塑化剂”污染风险防控的指导意见》规定油脂类食品DBP和DEHP最大残留量分别为0.3 mg/kg和1.5 mg/kg。本研究采用中国检科院质控样(QC-CO-705)进行数据准确性分析, DBP和DEHP实测值分别为2.65 mg/kg和1.64 mg/kg, 其中DBP的特性值为2.73 mg/kg, 特性值区间为2.64~3.00 mg/kg, DEHP特性值为1.65 mg/kg, 特性值区间为1.33~1.98 mg/kg, 质控回收率分别为97.07%和99.39%, 表明该方法准确可靠, 可应用于样品的检测分析。
本研究油茶籽油样品中的DBP和DEHP结果同见表3, 其中有10批次样品DBP超限量, 问题率为34.48%, 含量范围为0.43~12.90 mg/kg, 16批次样品DEHP含量大于0.5 mg/kg, 检出率为55.17 %, 含量范围为0.57~9.69 mg/kg, 其中有6批次超限量, 问题率为20.69%。从生产工艺的角度来看, 水酶法特级、超临界CO₂萃取一级、鲜籽初榨特级油茶籽油DBP和DEHP检出率偏高, 个别样品DBP超限量几十倍, 而压榨一级的检出率较低, 由此看出, 油茶籽油塑化剂的污染风险与原料、塑料制品的接触、加工工艺等综合因素相关, 近几年来油茶籽油中DBP和DEHP污染情况一直没有得到显著改观, 这与目前我国主要使用DBP和DEHP作为食品塑料包装材料中增塑剂的现状相符合[31], 也说明目前油茶籽油加工企业对控制塑化剂的污染风险有待进一步加强。
2.4 风险评估
油茶籽油中污染物的膳食暴露评估结果见表5, 由表5中可知, 成年女性居民每日通过食用油茶籽油摄入DBP、DEHP、3-MCPDE和GE的平均暴露量范围为0.66~0.75 μg/(kg·BW), 男性为0.56~0.63 μg/(kg·BW), 平均暴露水平远低于TDI值, 女性DBP、DEHP和3-MCPDE暴露风险范围为1.32%~37.37%, 男性为1.12%~31.68%, 其中3-MCPDE暴露风险为最高, 但均小于100%, 按照膳食推荐摄入量, 居民通过油茶籽油摄入上述污染物对人体造成危害的可能性很小。采用MOE来评估GE的膳食暴露风险发现, 男性居民MOE值高于女性, 但两者MOE值均小于10000, 表示健康风险需要引起关注。同时, 植物油经过高温烹调会增加3-MCPDE和GE的污染风险, 居民因不同饮食习惯通过加工食品也可能会引入3-MCPDE和GE的污染。因此, 对油茶籽油中DBP、DEHP、3-MCPDE和GE的暴露风险仍然不能放松警惕, 除了要加强风险监管监测其真实含量, 还应控制生产加工过程中的污染物含量。
3 结论
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本研究通过对29批次江西省市售油茶籽油的污染物检测发现, 有23批次样品存在不同程度的3-MCPDE和GE检出, 有21批次样品存在不同程度的DBP和DEHP检出, 其中3-MCPDE检出率最高达75.86%, 含量范围为0.11~4.52 mg/kg, GE的问题率最高达44.83%, 含量范围为0.13~11.76 mg/kg, DBP问题率为34.48%, 含量范围为0.43~12.90 mg/kg, DEHP检出率为55.17%, 含量范围为0.57~9.69 mg/kg。由此可见, 市场上的油茶籽油存在一定程度的3-MCPDE、GE及PAEs污染风险, 但本研究未收集样品的具体工艺参数如脱臭温度、脱色剂类型等, 结论可能存在偏差, 后续研究将增加企业生产工艺调研, 以更精准定位污染源。
此外, 健康风险评估表明, 消费者通过油茶籽油摄入上述污染物存在一定的潜在风险, 若考虑其他食品的叠加暴露风险, 实际健康风险可能更高。本研究系统性揭示了江西省油茶籽油中DBP、DEHP、3-MCPDE和GE的污染情况, 提出差异化控制策略, 初步构建了健康风险评估模型, 为后续进一步扩大样本量以建立全国性污染数据及膳食暴露研究提供数据支持, 为油茶籽油质量安全标准的修订提供依据, 为企业工艺优化提供指导, 为质量监管提供思路。
基金
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  • 江西省市场监督管理局科技项目(GSJK202309)
  • 江西省重点研发计划项目(20233BBF64002)
  • 国家市场监督管理总局科技计划项目(2023MK073)
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20250121003
  • 接收时间：2025-01-21
  • 首发时间：2025-07-15
  • 出版时间：2025-05-25
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  • 收稿日期：2025-01-21
基金
江西省市场监督管理局科技项目(GSJK202309)
江西省重点研发计划项目(20233BBF64002)
国家市场监督管理总局科技计划项目(2023MK073)
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    赣州市综合检验检测院, 赣州 341000

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* 陈玮玲(1992—), 女, 工程师, 主要研究方向为食品质量与安全。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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