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Article(id=1152687437227672118, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1152687434774000221, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20241217002, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1734364800000, receivedDateStr=2024-12-17, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1752751700931, onlineDateStr=2025-07-17, pubDate=1747238400000, pubDateStr=2025-05-15, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1752751700931, onlineIssueDateStr=2025-07-17, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1752751700931, creator=13701087609, updateTime=1752751700931, updator=13701087609, issue=Issue{id=1152687434774000221, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='9', 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=1752751700342, creator=13701087609, updateTime=1756708585928, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1169283815848555430, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1152687434774000221, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1169283815848555431, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1152687434774000221, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=99, endPage=105, ext={EN=ArticleExt(id=1152687437621936697, articleId=1152687437227672118, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Research on rapid screening method for volatile components of lubricating oil in edible oil based on headspace-gas chromatography-mass spectrometry, columnId=1152687436694995508, journalTitle=Journal of Food Safety & Quality, columnName=Special Topic: Grain and Oil Processing and Quality Safety, runingTitle=null, highlight=null, articleAbstract=

Objective To establish a method for determining the volatile components of lubricating oil mixed in edible oil by headspace-gas chromatography-mass spectrometry. Methods The 1.0 g oil sample was directly taken into a 10 mL headspace bottle, then capped and sealed. Headspace-gas chromatography-mass spectrometry analysis was carried out at 90 ℃ equilibration for 20 min. Qualitative analysis was performed on 5 kinds of compounds: 4-methyl-2-pentanol, isooctanol, nonane, undecane and dodecane, while quantitative analysis was performed on isooctanol, nonane, undecane, and dodecane. Results The 4 kinds of quantitative compounds showed good linear relationships within the range of 0.5-8.0 mg/kg, and the correlation coefficients were all above 0.9980. Soybean oil was used as the sample for the spike recovery experiment. The recoveries of nonane, isooctanol, undecane, dodecane were 91.5%-98.2%, 81.9%-92.7%, 92.8%-94.6%, 89.3%-93.7% respectively and the relative standard deviations were all less than 10%. In the 5 kinds of edible oils: Soybean oil, peanut oil, rapeseed oil, corn oil and sunflower seed oil, the limits of detection of nonane, isooctanol, undecane, dodecane were 0.006-0.013 mg/kg, 0.016-0.045 mg/kg, 0.011-0.020 mg/kg, 0.020-0.036 mg/kg respectively. Conclusion This method has the advantages of simple operation and rapid detection, and does not have high requirements for the instrument, which can be carried out in general laboratories, and is suitable for the screening of trace lubricating oil contamination in edible oil.

, correspAuthors=Hua-Liang LIU, 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=Xian-Xian GU, Yan FANG, Hua-Liang LIU), CN=ArticleExt(id=1152687450666222551, articleId=1152687437227672118, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=基于顶空-气相色谱-质谱法的食用油中润滑油挥发性组分快速筛查方法研究, columnId=1152687437265420855, journalTitle=食品安全质量检测学报, columnName=本期专题：粮油加工与质量安全, runingTitle=null, highlight=null, articleAbstract=

目的 建立顶空-气相色谱-质谱法测定食用油中混入的润滑油挥发性组分的方法。方法 直接取1.0 g油样于10 mL顶空瓶中加盖密封, 在90 ℃平衡20 min的条件下顶空进样进行气相色谱-质谱仪检测, 以4-甲基-2-戊醇、异辛醇、壬烷、十一烷和十二烷5种化合物定性, 以异辛醇、壬烷、十一烷和十二烷4种化合物定量。结果 4种定量化合物在0.5~8.0 mg/kg范围内线性关系良好, 相关系数均大于0.9980。以大豆油为加标实验样品, 壬烷、异辛醇、十一烷和十二烷的加标回收率分别为91.5%~98.2%、81.9%~92.7%、92.8%~94.6%、89.3%~93.7%, 相对标准偏差均小于10%。在大豆油、花生油、菜籽油、玉米油、葵花籽油5种食用油中壬烷、异辛醇、十一烷和十二烷的检出限分别为0.006~0.013 mg/kg、0.016~0.045 mg/kg、0.011~0.020 mg/kg和0.020~0.036 mg/kg。结论 该方法具有操作简单、检测快速等优势, 对仪器要求不高, 一般实验室均能开展, 适用于食用油中微量润滑油污染的筛查。

, correspAuthors=刘华良, authorNote=null, correspAuthorsNote=
* 刘华良(1973—), 男, 研究员, 主要研究方向为卫生理化研究。E-mail:
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顾显显(1994—), 女, 主管技师, 主要研究方向为水质及食品检测。E-mail:

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Jiangsu Provincial Center for Disease Control and Prevention, Nanjing 210009, China), AuthorCompanyExt(id=1169272675433194395, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1152687437227672118, companyId=1169272675412222872, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.江苏省疾病预防控制中心, 南京 210009)]), AuthorCompany(id=1169272675508691868, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1152687437227672118, xref=null, ext=[AuthorCompanyExt(id=1169272675517080477, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1152687437227672118, companyId=1169272675508691868, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2. Nanjing Gulou Provincial Center for Disease Control and Prevention, Nanjing 210003, China), AuthorCompanyExt(id=1169272675521274782, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1152687437227672118, companyId=1169272675508691868, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.南京市鼓楼区疾病预防控制中心, 南京 210003)])], figs=[ArticleFig(id=1169272676976698294, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1152687437227672118, language=EN, label=Fig.1, caption=Full scan spectra of lubricating oil and soybean oil by gas chromatography-mass spectrometry, figureFileSmall=6i50JTiL40Fti2w6dP/6jg==, figureFileBig=GvTaDJ13QfXk8LKmdz7FIg==, tableContent=null), ArticleFig(id=1169272677085750199, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1152687437227672118, language=CN, label=图1, caption=润滑油和大豆油气相色-谱质谱仪的全扫描图谱, figureFileSmall=6i50JTiL40Fti2w6dP/6jg==, figureFileBig=GvTaDJ13QfXk8LKmdz7FIg==, tableContent=null), ArticleFig(id=1169272677148664760, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1152687437227672118, language=EN, label=Fig.2, caption=Effects of different volumes of n-hexane on the peak areas of 4 kinds of compounds, figureFileSmall=UndP0DYQKXv3G0+lGQRnzA==, figureFileBig=ZeZLP/1kySdARy8U8ssKJg==, tableContent=null), ArticleFig(id=1169272677203190713, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1152687437227672118, language=CN, label=图2, caption=不同体积正己烷对4种化合物峰面积的影响

注: 不同小写字母表示不同正己烷体积的同一化合物峰面积差异显著(P<0.05)。

, figureFileSmall=UndP0DYQKXv3G0+lGQRnzA==, figureFileBig=ZeZLP/1kySdARy8U8ssKJg==, tableContent=null), ArticleFig(id=1169272677261910970, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1152687437227672118, language=EN, label=Fig.3, caption=Peak areas of 4 kinds of target compounds at different headspace equilibrium times (a) and equilibrium temperatures (b), figureFileSmall=t0BPIvvagBbxNc/hB67Qcg==, figureFileBig=hiPquNrWzINpem9woPOHUA==, tableContent=null), ArticleFig(id=1169272677312242619, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1152687437227672118, language=CN, label=图3, caption=4种目标化合物在不同顶空平衡时间(a)以及平衡温度(b)下的峰面积, figureFileSmall=t0BPIvvagBbxNc/hB67Qcg==, figureFileBig=hiPquNrWzINpem9woPOHUA==, tableContent=null), ArticleFig(id=1169272677362574268, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1152687437227672118, language=EN, label=Table 1, caption=

Ion information for each compound

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物 定量离子 定性离子
4-甲基-2-戊醇 / 87,69,45,43
壬烷 57 85,43,41
异辛醇 57 84,70,43
十一烷 57 85,71,43
十二烷 57 85,71,43
), ArticleFig(id=1169272677446460349, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1152687437227672118, language=CN, label=表1, caption=

各化合物离子信息

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物 定量离子 定性离子
4-甲基-2-戊醇 / 87,69,45,43
壬烷 57 85,43,41
异辛醇 57 84,70,43
十一烷 57 85,71,43
十二烷 57 85,71,43
), ArticleFig(id=1169272677538735038, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1152687437227672118, language=EN, label=Table 2, caption=

ME of 4 kinds of target compounds in different edible oil sample matrices

, figureFileSmall=null, figureFileBig=null, tableContent=
目标化合物名称 基质 回归方程 相关系数(r) 斜率 ME/%
壬烷 溶剂 Y=16520X-1493 0.9996 Ss: 16520 /
大豆油 Y=16910X-1604 0.9983 Sm: 16910 2.4
花生油 Y=15110X+723 0.9981 Sm: 15110 -8.5
菜籽油 Y=14790X+3707 0.9993 Sm: 14790 -11.0
玉米油 Y=17450X+81 0.9990 Sm: 17450 5.6
葵花籽油 Y=16880X-810 0.9995 Sm: 16880 2.2
异辛醇 溶剂 Y=3304X-839 0.9991 Ss: 3304 /
大豆油 Y =1154X-347 0.9982 Sm: 1154 -65.0
花生油 Y =940X+252 0.9985 Sm: 940 -72.0
菜籽油 Y=911X+221 0.9994 Sm: 911 -72.0
玉米油 Y=1161X-214 0.9993 Sm: 1161 -65.0
葵花籽油 Y=1004X-172 0.9996 Sm: 1004 -70.0
十一烷 溶剂 Y=6794X-1796 0.9993 Ss: 6794 /
大豆油 Y=5102X-1993 0.9982 Sm: 5102 -25.0
花生油 Y=3922X+544 0.9981 Sm: 3922 -42.0
菜籽油 Y=3993X+596 0.9991 Sm: 3993 -41.0
玉米油 Y=5736X-1495 0.9990 Sm: 5736 -16.0
葵花籽油 Y=4842X-1115 0.9994 Sm: 4842 -29.0
十二烷 溶剂 Y=4453X-1564 0.9992 Ss: 4453 /
大豆油 Y=2430X-1011 0.9984 Sm: 2430 -45.0
花生油 Y=1715X+411 0.9988 Sm: 1715 -61.0
菜籽油 Y=1666X+442 0.9992 Sm: 1666 -63.0
玉米油 Y=2653X-737 0.9994 Sm: 2653 -40.0
葵花籽油 Y=2025X-359 0.9991 Sm: 2025 -55.0
), ArticleFig(id=1169272677635204031, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1152687437227672118, language=CN, label=表2, caption=

4种目标化合物在不同食用油样品基质中的ME

, figureFileSmall=null, figureFileBig=null, tableContent=
目标化合物名称 基质 回归方程 相关系数(r) 斜率 ME/%
壬烷 溶剂 Y=16520X-1493 0.9996 Ss: 16520 /
大豆油 Y=16910X-1604 0.9983 Sm: 16910 2.4
花生油 Y=15110X+723 0.9981 Sm: 15110 -8.5
菜籽油 Y=14790X+3707 0.9993 Sm: 14790 -11.0
玉米油 Y=17450X+81 0.9990 Sm: 17450 5.6
葵花籽油 Y=16880X-810 0.9995 Sm: 16880 2.2
异辛醇 溶剂 Y=3304X-839 0.9991 Ss: 3304 /
大豆油 Y =1154X-347 0.9982 Sm: 1154 -65.0
花生油 Y =940X+252 0.9985 Sm: 940 -72.0
菜籽油 Y=911X+221 0.9994 Sm: 911 -72.0
玉米油 Y=1161X-214 0.9993 Sm: 1161 -65.0
葵花籽油 Y=1004X-172 0.9996 Sm: 1004 -70.0
十一烷 溶剂 Y=6794X-1796 0.9993 Ss: 6794 /
大豆油 Y=5102X-1993 0.9982 Sm: 5102 -25.0
花生油 Y=3922X+544 0.9981 Sm: 3922 -42.0
菜籽油 Y=3993X+596 0.9991 Sm: 3993 -41.0
玉米油 Y=5736X-1495 0.9990 Sm: 5736 -16.0
葵花籽油 Y=4842X-1115 0.9994 Sm: 4842 -29.0
十二烷 溶剂 Y=4453X-1564 0.9992 Ss: 4453 /
大豆油 Y=2430X-1011 0.9984 Sm: 2430 -45.0
花生油 Y=1715X+411 0.9988 Sm: 1715 -61.0
菜籽油 Y=1666X+442 0.9992 Sm: 1666 -63.0
玉米油 Y=2653X-737 0.9994 Sm: 2653 -40.0
葵花籽油 Y=2025X-359 0.9991 Sm: 2025 -55.0
), ArticleFig(id=1169272677727478720, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1152687437227672118, language=EN, label=Table 3, caption=

Results of spiking recovery experiments for 4 kinds of target compounds in soybean oil samples (n=6)

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物 本底值/(mg/kg) 加标值/(mg/kg) 测得值/(mg/kg) 平均
回收率/%		 RSDs/%
壬烷 / 1.0 0.915 91.5 5.0
/ 2.0 1.964 98.2 2.1
/ 5.0 4.821 96.3 6.9
异辛醇 / 1.0 0.927 92.7 8.3
/ 2.0 1.638 81.9 6.8
/ 5.0 4.483 89.7 6.1
十一烷 / 1.0 0.938 93.8 5.0
/ 2.0 1.892 94.6 4.1
/ 5.0 4.640 92.8 6.3
十二烷 / 1.0 0.937 93.7 6.9
/ 2.0 1.786 89.3 6.4
/ 5.0 4.505 90.1 7.1
), ArticleFig(id=1169272677823947713, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1152687437227672118, language=CN, label=表3, caption=

4种目标化合物在大豆油样品中的加标回收实验结果(n=6)

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物 本底值/(mg/kg) 加标值/(mg/kg) 测得值/(mg/kg) 平均
回收率/%		 RSDs/%
壬烷 / 1.0 0.915 91.5 5.0
/ 2.0 1.964 98.2 2.1
/ 5.0 4.821 96.3 6.9
异辛醇 / 1.0 0.927 92.7 8.3
/ 2.0 1.638 81.9 6.8
/ 5.0 4.483 89.7 6.1
十一烷 / 1.0 0.938 93.8 5.0
/ 2.0 1.892 94.6 4.1
/ 5.0 4.640 92.8 6.3
十二烷 / 1.0 0.937 93.7 6.9
/ 2.0 1.786 89.3 6.4
/ 5.0 4.505 90.1 7.1
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基于顶空-气相色谱-质谱法的食用油中润滑油挥发性组分快速筛查方法研究
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顾显显 1 , 方燕 2 , 刘华良 1, *
食品安全质量检测学报 | 本期专题：粮油加工与质量安全 2025,16(9): 99-105
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食品安全质量检测学报 | 本期专题：粮油加工与质量安全 2025, 16(9): 99-105
基于顶空-气相色谱-质谱法的食用油中润滑油挥发性组分快速筛查方法研究
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顾显显1 , 方燕2, 刘华良1, *
作者信息
  • 1.江苏省疾病预防控制中心, 南京 210009
  • 2.南京市鼓楼区疾病预防控制中心, 南京 210003

    • 顾显显(1994—), 女, 主管技师, 主要研究方向为水质及食品检测。E-mail:

通讯作者:

* 刘华良(1973—), 男, 研究员, 主要研究方向为卫生理化研究。E-mail:
Research on rapid screening method for volatile components of lubricating oil in edible oil based on headspace-gas chromatography-mass spectrometry
Xian-Xian GU1 , Yan FANG2, Hua-Liang LIU1, *
Affiliations
  • 1. Jiangsu Provincial Center for Disease Control and Prevention, Nanjing 210009, China
  • 2. Nanjing Gulou Provincial Center for Disease Control and Prevention, Nanjing 210003, China
出版时间: 2025-05-15 doi: 10.19812/j.cnki.jfsq11-5956/ts.20241217002
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摘要
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目的 建立顶空-气相色谱-质谱法测定食用油中混入的润滑油挥发性组分的方法。方法 直接取1.0 g油样于10 mL顶空瓶中加盖密封, 在90 ℃平衡20 min的条件下顶空进样进行气相色谱-质谱仪检测, 以4-甲基-2-戊醇、异辛醇、壬烷、十一烷和十二烷5种化合物定性, 以异辛醇、壬烷、十一烷和十二烷4种化合物定量。结果 4种定量化合物在0.5~8.0 mg/kg范围内线性关系良好, 相关系数均大于0.9980。以大豆油为加标实验样品, 壬烷、异辛醇、十一烷和十二烷的加标回收率分别为91.5%~98.2%、81.9%~92.7%、92.8%~94.6%、89.3%~93.7%, 相对标准偏差均小于10%。在大豆油、花生油、菜籽油、玉米油、葵花籽油5种食用油中壬烷、异辛醇、十一烷和十二烷的检出限分别为0.006~0.013 mg/kg、0.016~0.045 mg/kg、0.011~0.020 mg/kg和0.020~0.036 mg/kg。结论 该方法具有操作简单、检测快速等优势, 对仪器要求不高, 一般实验室均能开展, 适用于食用油中微量润滑油污染的筛查。

顶空-气相色谱-质谱法  /  食用油  /  润滑油  /  挥发性组分

Objective To establish a method for determining the volatile components of lubricating oil mixed in edible oil by headspace-gas chromatography-mass spectrometry. Methods The 1.0 g oil sample was directly taken into a 10 mL headspace bottle, then capped and sealed. Headspace-gas chromatography-mass spectrometry analysis was carried out at 90 ℃ equilibration for 20 min. Qualitative analysis was performed on 5 kinds of compounds: 4-methyl-2-pentanol, isooctanol, nonane, undecane and dodecane, while quantitative analysis was performed on isooctanol, nonane, undecane, and dodecane. Results The 4 kinds of quantitative compounds showed good linear relationships within the range of 0.5-8.0 mg/kg, and the correlation coefficients were all above 0.9980. Soybean oil was used as the sample for the spike recovery experiment. The recoveries of nonane, isooctanol, undecane, dodecane were 91.5%-98.2%, 81.9%-92.7%, 92.8%-94.6%, 89.3%-93.7% respectively and the relative standard deviations were all less than 10%. In the 5 kinds of edible oils: Soybean oil, peanut oil, rapeseed oil, corn oil and sunflower seed oil, the limits of detection of nonane, isooctanol, undecane, dodecane were 0.006-0.013 mg/kg, 0.016-0.045 mg/kg, 0.011-0.020 mg/kg, 0.020-0.036 mg/kg respectively. Conclusion This method has the advantages of simple operation and rapid detection, and does not have high requirements for the instrument, which can be carried out in general laboratories, and is suitable for the screening of trace lubricating oil contamination in edible oil.

headspace-gas chromatography-mass spectrometry  /  edible oil  /  lubricating oil  /  volatile components
顾显显, 方燕, 刘华良. 基于顶空-气相色谱-质谱法的食用油中润滑油挥发性组分快速筛查方法研究. 食品安全质量检测学报, 2025 , 16 (9) : 99 -105 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241217002
Xian-Xian GU, Yan FANG, Hua-Liang LIU. Research on rapid screening method for volatile components of lubricating oil in edible oil based on headspace-gas chromatography-mass spectrometry[J]. Journal of Food Safety & Quality, 2025 , 16 (9) : 99 -105 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241217002
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0 引言
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食品安全与社会稳定发展密切相关, 当食品安全出现问题时会威胁公众健康, 破坏社会稳定。随着生活水平的提高, 人民对食品安全问题也越发关注。2024年7月“中储粮油罐车混装食用油”事件也暴露出我国面临的食品安全问题的严峻性[1-2]。食用油作为日常生活的必需品, 保障其质量安全尤为重要。煤制油是指以煤炭为原料经过各种化学反应形成多碳化合物, 再进行重整、裂化、合成后的矿物油产品, 如柴油、汽油、煤油、润滑油等[3]。其主要化学成分是C10~C50的烃类化合物, 包括直链、支链和烷基取代的环状饱和烷烃(mineral oil saturated hydrocarbons, MOSH)以及烷基取代的芳香烃(mineral oil aromatic hydrocarbons, MOAH)两类[4]。欧洲食品安全局(European Food Safety Authority, EFSA)在2012年发布的评估报告[5]中指出, MOSH几乎存在于所有食品中。有研究表明, 矿物油经膳食摄入后易在人体内长期蓄积, 是人体内蓄积量最大的污染物, 而芳香烃类矿物油更是具有致突变性, 含有3个以上苯环的芳香烃还有遗传致癌性[6-7]。本研究所涉及的5种化合物都属于MOSH。其中4-甲基-2-戊醇、十一烷、十二烷因其润滑性、黏度特性和热稳定性, 常被用作润滑油的基础油成分, 广泛应用于多个领域; 而壬烷在润滑油中主要作为添加剂或溶剂, 能调节润滑油的黏度, 提升其性能, 使其更适合在低温低黏度条件下使用。异辛醇既可以做基础油组分也可以充当添加剂及溶剂, 能够提升润滑油的抗氧化、抗腐蚀性能, 还能改善润滑油的生物降解, 减少对环境的影响。
氢火焰离子化检测器因其对碳响应完全一致的特点成为矿物油定量测定的首选方法。目前, 在线高效液相色谱-气相色谱氢火焰离子化检测器法(high performance liquid chromatography-gas chromatography-hydrogen flame ionization detector, HPLC-GC-FID)和离线固相萃取气相色谱氢火焰离子化检测器法(solid phase extraction-gas chromatography-hydrogen flame ionization detector, SPE-GC-FID)[8-13]是最常用的矿物油分析方法。HPLC-GC通过HPLC与GC的Y接口技术实现在线净化、富集, 有效提高了矿物油的分离和检出限, 且干扰较少; 而离线SPE主要是利用银渍硅胶和氧化铝复合净化柱对样品进行净化、富集, 再配合程序升温气化进样口(programmable temperature vaporizer, PTV)进行分析。此外, 刘亮等[14]采用气相色谱-质谱法检测矿物油在肉鸡体内的残留量变化, 但是由于矿物油结构信息不足、没有共同的离子碎片也无法有效地分别定量MOSH和MOAH; 钱沙沙等[15]采用全二维气相色谱法测定食品接触用纸制品中饱和烃矿物油的迁移量, 全二维气相色谱利用化合物极性和沸点的不同, 进行二次分离, 能够对一维气相色谱无法解决的碳混合物进行有效地分离和定量[16]。同时有研究表明, 在相同分析时间和条件下, 全二维的峰容量可达到一维色谱的10倍[17]。
但由于HPLC-GC-FID、SPE-GC-FID以及全二维气相色谱法或需配备大体积进样系统或因仪器价格昂贵, 普及率不高, 大部分实验室均不具备可行性。故本研究尝试用常见的顶空-气相色谱-质谱法对食用油中混入的微量润滑油主要成分进行定性定量分析, 作为食用油被润滑油污染的初步筛查手段。
1 材料与方法
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1.1 材料、试剂与仪器
金龙鱼大豆油、鲁花花生油、福临门菜籽油、福临门玉米油、金龙鱼葵花籽油: 均从超市购入; 润滑油(太行润滑煤制油, 山西潞安太行润滑科技股份有限公司)。
十一烷(纯度99.9%)、十二烷(纯度99.6%)、壬烷(纯度99.5%)、正己烷(色谱纯)(上海安谱公司); 异辛醇(纯度99.0%, 上海阿拉丁公司)。
7890B-5977A气相色谱质谱仪(配全自动顶空进样器7697A、10 mL顶空瓶带聚四氟乙烯瓶盖)、DB-5MS色谱柱(30 m×0.25 mm, 0.25 μm)(美国安捷伦公司); MA204万分之一天平(瑞士梅特勒-托利多公司)。
1.2 方法
1.2.1 样品前处理
称取1 g(精确至0.01 g)样品于10 mL顶空瓶中加盖密封后水平摇动混匀, 待测。待测样品应在洁净环境中室温保存, 取样前要充分混匀样品, 取样后要及时密封好样品; 注意样品的有效期和保存期, 防止样品酸败变质, 影响实验结果。
1.2.2 标准溶液配制
(1)标准储备液的配制
分别准确称取0.1000 g壬烷、异辛醇、十一烷、十二烷于4个10 mL容量瓶中, 用正己烷定容至刻度, 混匀。得到壬烷、异辛醇、十一烷、十二烷单标储备液质量浓度均为10000 mg/L。
(2)混合标准使用液的配制
分别准确吸取0.1 mL壬烷、异辛醇、十一烷、十二烷单标储备液于10 mL容量瓶中, 用正己烷定容至刻度, 混匀。得到4种化合物混合标准使用液质量浓度为100 mg/L。
(3)纯溶剂标准曲线的配制
准确吸取1.0 mL正己烷于10 mL顶空瓶中, 平行6份, 分别加入混合标准使用液0、5、10、20、40、80 µL, 加盖密封, 配制成含壬烷、异辛醇、十一烷、十二烷浓度均为0、0.5、1.0、2.0、4.0、8.0 mg/kg的纯溶剂标准系列。保持顶空样品瓶直立, 做水平圆周振摇, 使其充分混合。振摇过程中溶剂不能接触到密封垫, 若有接触需重新配制。
(4)基质标准工作曲线的配制
称取1 g(精确至0.01 g)空白基质样品(不含目标物的食用油样品)于10 mL顶空瓶中, 平行6份, 分别加入混合标准使用液0、5、10、20、40、80 µL, 加盖密封, 配制成含壬烷、异辛醇、十一烷、十二烷浓度均为0、0.5、1.0、2.0、4.0、8.0 mg/kg的基质标准系列。保持顶空样品瓶直立, 做水平圆周振摇, 使物质充分混合。振摇过程中食用油不能接触到密封垫, 若有接触需重新配制。
1.2.3 空白样品制备
将大豆油、花生油、菜籽油、玉米油、葵花籽油5种代表性基质样品在实验室条件下经90 ℃加热30 min并通入干燥氮气处理[18], 确保本底不含待测目标化合物干扰后作为空白样品。
1.2.4 仪器条件
(1)气相色谱条件
DB-5MS色谱柱(30 m×0.25 mm, 0.25 μm); 柱温采用程序升温: 40 ℃保持3 min, 以10 ℃/min升至220 ℃保持1 min; 进样口温度180 ℃; 分流比20:1; 载气为高纯氦气, 柱流量为1.0 mL/min。
(2)质谱条件
电子轰击源(electron impact ionization, EI), 离子源230 ℃, 四极杆150 ℃, 传输线280 ℃。采集模式: 选择离子模式(selected ion monitor, SIM), 溶剂延迟5 min, 增益因子1.0, 各化合物离子信息见表1。
(3)顶空进样器条件
炉温90 ℃, 定量环110 ℃, 传输线130 ℃; 顶空瓶平衡20 min, 加压1 min, 进样时间0.5 min。
1.2.5 定性及定量分析
按照上述条件对样品进行测定, 根据保留时间定性, 外标法定量。以各目标化合物的浓度为横坐标(X, mg/kg), 峰面积为纵坐标(Y)绘制基质标准曲线, 通过基质标准曲线来计算样品中各目标化合物的含量。
1.3 数据处理
本研究前处理条件优化均为3次平行样品测定, 方法学验证为6次平行测定。顶空-气相色谱-质谱联用仪测得的数据通过安捷伦MassHunter Workstation工作站进行标准曲线绘制及线性方程计算。利用WPS Office Excel 2019软件对数据进行统计分析和制作表格, 采用Origin 2019b软件绘图。
2 结果与分析
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2.1 目标化合物的确定
选取市面上某润滑油产品以及常用的5种食用油(大豆油、花生油、菜籽油、玉米油、葵花籽油)作为实验对象, 分别称取1 g样品于10 mL顶空瓶中, 加盖密封, 用气相色谱-质谱仪进行全扫描分析。通过比较润滑油与5种食用油的全扫描图谱, 选出润滑油中含有而5种食用油中均不含有的化合物作为润滑油污染的标志物。本研究选出了壬烷、异辛醇、十一烷和十二烷4种可定量的化合物, 4-甲基-2-戊醇则因缺少标准品而作为定性化合物。润滑油中还含有其他一些化合物, 且在5种食用油中也未检出, 但因其含量较低不予考虑。其中润滑油和大豆油的全扫描图谱见图1。
2.2 正己烷体积对响应的影响
以大豆油为实验对象, 分别称取1 g大豆油于6个10 mL顶空瓶, 加入50 µL质量浓度为100 mg/L的混合标准使用液, 再分别加入不同体积的正己烷, 加盖密封后水平摇动混匀进行测定。考察在油样中加入正己烷以增加油样的流动性和挥发性是否能提高化合物的响应。结果表明(图2), 当1 g试样中正己烷体积大于80 µL时, 壬烷和十一烷峰面积呈下降趋势; 当正己烷体积达到500 µL时, 异辛醇和十二烷峰面积也呈下降趋势。研究结果表明在试样中加入正己烷并不能增加4种化合物的响应, 还会降低其峰面积, 这可能是正己烷的大量挥发反而占据了顶空气大部分体积, 稀释了目标化合物的浓度。其产生的负效应大于上层顶空体积缩小的正效应。故为了实验的准确性在配制工作曲线时应尽量控制加入的正己烷体积均在80 µL以内, 否则基质曲线高浓度点的峰面积就会偏低而影响线性。
2.3 顶空平衡温度与时间的优化
以大豆油为实验对象, 取1 g大豆油于10 mL顶空瓶中, 加入50 µL质量浓度为100 mg/L的混合标准使用液后考察不同平衡温度和时间对目标化合物峰面积的影响。先考察80 ℃时不同平衡时间(10、20、30、40、50 min)下目标化合物峰面积情况。结果发现随着时间的增加, 峰面积增加, 20 min时趋于稳定, 40 min后又有所下降(图3a)。为了减少检测时间提高效率, 故选择20 min的平衡时间。再考察20 min下不同平衡温度(50、60、70、80、90 ℃)时目标化合物峰面积情况。结果表明, 在相同平衡时间下, 随着温度增加, 目标化合物峰面积随之增加, 90 ℃时达到峰值, 考虑到方法的灵敏度需要, 故选择90 ℃的平衡温度。其次, 从图3b中的面积增长趋势来看, 温度继续升高各化合物峰面积还会进一步增加, 但是考虑到温度过高可能会影响顶空瓶瓶盖的气密性和耐热性, 甚至导致更多挥发性物质及热分解产物[19-20]的干扰, 故本研究不再考察更高的顶空温度。4种目标化合物在不同顶空平衡时间以及平衡温度下的峰面积见图3。
2.4 基质效应考察
目前, 在顶空进样的方法学研究中, 基质效应(matrix effects, ME)越来越被学者所重视。有相关研究表明, 样品基质的存在及量的变化确实会影响实验的结果[21-23]。按1.2.2分别配制纯溶剂标准曲线和5种食用油基质匹配的标准工作曲线进行测定。根据每种目标化合物在纯溶剂标准曲线和5种食用油基质匹配的标准工作曲线中获得的线性方程, 按公式(1)计算ME[24-25]。当ME<0时表示基质抑制效应, ME>0时表示基质增强效应, 其中当ME的绝对值为0%~20%时为弱ME, 20%~50%时为中等ME, ME>50%时为强ME[26-29]。
ME/%=($\frac{{{S}_{\text{m}}}}{{{S}_{\text{s}}}}$–1)×100%
式中: Sm和Ss分别表示基质匹配标准工作曲线和纯溶剂标准曲线的斜率。
表2为4种目标化合物在不同食用油样品基质中的ME情况。由表2可以看出, 壬烷在5种食用油中均呈弱ME, 异辛醇均呈强ME, 十一烷除在玉米油中均呈中等ME, 十二烷则在大豆油和玉米油中呈中等ME, 在另外3种食用油中呈强ME。故异辛醇、十一烷和十二烷在不同食用油样品中的ME是不可忽略的。因此, 在检测工作中要注意ME对于结果的影响, 尤其当测定值处于限值时, 要尽量采取基质配标等方法消除ME[30]。
2.5 线性范围、回归方程和检出限
在0.5~8.0 mg/kg的线性范围内, 4种目标化合物在5种常用食用油中的回归方程见表2, 线性关系良好, 相关系数均在0.9980以上。以3倍信噪比计算, 壬烷在大豆油、花生油、菜籽油、玉米油、葵花籽油中的检出限分别为0.006、0.010、0.010、0.013、0.010 mg/kg, 异辛醇的检出限分别为0.045、0.023、0.029、0.016、0.022 mg/kg, 十一烷的检出限分别为0.013、0.011、0.012、0.013、0.020 mg/kg, 十二烷的检出限分别为0.025、0.021、0.020、0.028、0.036 mg/kg。
2.6 回收率和精密度
根据上述样品处理方法, 选取大豆油作为样品进行加标回收实验, 加标浓度为1.0、2.0、5.0 mg/kg, 每个浓度水平6个平行, 结果见表3。在低、中、高3个加标浓度水平下4种化合物的回收率范围在81.9%~98.2%, RSDs范围在2.1%~8.3%, 均符合检测要求。
2.7 实际食用油样品的检测
根据上述样品处理方法, 对从超市购入的金龙鱼大豆油、鲁花花生油、福临门菜籽油、福临门玉米油、金龙鱼葵花籽油5种日常食用油样品进行检测。结果显示5种食用油样品中均未检出4-甲基-2-戊醇、异辛醇、壬烷、十一烷和十二烷。
3 结论
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本研究采用顶空-气相色谱-质谱法对食用油中混入的润滑油主要成分进行定性定量分析, 作为润滑油污染的初步筛查手段。方法较在线HPLC-GC-FID、离线SPE-GC-FID和二维气相更为简单快捷, 对仪器要求不高, 一般实验室均能开展。在大豆油、花生油、菜籽油、玉米油、葵花籽油5种食用油中可定量的壬烷、异辛醇、十一烷和十二烷检出限分别为0.006~0.013 mg/kg、0.016~0.045 mg/kg、0.011~0.020 mg/kg和0.020~0.036 mg/kg, 均低于0.1 ppm。对于30 t的油罐车来说, 混入3 L润滑油就能被本方法检测到, 足够满足食用油中微量润滑油的污染筛查, 同时其加标回收率和精密度均能满足要求。不足的是, 本研究仅选取了某润滑油产品中的5种化合物作为润滑油污染标志物, 可能存在一定的局限性, 需进一步扩大润滑油污染标志物的组分范围, 以便为后续研究提供改进方向。
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2025年第16卷第9期
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20241217002
  • 接收时间：2024-12-17
  • 首发时间：2025-07-17
  • 出版时间：2025-05-15
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  • 收稿日期：2024-12-17
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    1.江苏省疾病预防控制中心, 南京 210009
    2.南京市鼓楼区疾病预防控制中心, 南京 210003

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* 刘华良(1973—), 男, 研究员, 主要研究方向为卫生理化研究。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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