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Article(id=1151881494868931009, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1151881493552394994, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20241112002, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1731340800000, receivedDateStr=2024-11-12, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1752559549299, onlineDateStr=2025-07-15, pubDate=1748102400000, pubDateStr=2025-05-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1752559549299, onlineIssueDateStr=2025-07-15, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1752559549299, creator=13701087609, updateTime=1752559549299, 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=173, endPage=178, ext={EN=ArticleExt(id=1151923894693802708, articleId=1151881494868931009, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Identification of morpholine in morpholine fatty acid salt fruit wax by gas chromatography, columnId=1151895322692776479, journalTitle=Journal of Food Safety & Quality, columnName=Special Topic: Analysis and Monitoring of Toxic and Harmful Substances in Food, runingTitle=null, highlight=null, articleAbstract=

Objective To establish a method for the identification of morpholine in morpholine fatty acid salt fruit wax by gas chromatography. Methods Morpholine fatty acid salt was hydrolyzed to morpholine using hydrochloric acid solution, and the pH of the solution was adjusted with sodium hydroxide acid solution. Detection was performed using gas chromatography-hydrogen flame ionization detector. Results The matrix effect of the method was 96.67%; there was no interference from sample blanks, reagent blanks, and standard solution blanks on the qualitative analysis of the target substance; the deviation of peak area for samples of different concentrations within 48 hours was within ±5%. The method was used to analyze the actual commercial samples, and 12 batches of samples were detected morpholine. Conclusion This method has the advantages of minimal interference, strong specificity, and good repeatability. The pretreatment process is simple and environmentally friendly, providing technical support for the identification of morpholine in morpholine fatty acid salt fruit wax.

, correspAuthors=Wei WANG, 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=Bei-Bei LI, Ju ZHANG, Wei WANG), CN=ArticleExt(id=1151923907129913383, articleId=1151881494868931009, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=气相色谱法鉴别吗啉脂肪酸盐果蜡中的吗啉, columnId=1151923892102197877, journalTitle=食品安全质量检测学报, columnName=专题：食品中有毒有害物质分析与监测, runingTitle=null, highlight=null, articleAbstract=

目的 建立气相色谱法鉴别吗啉脂肪酸盐果蜡中的吗啉。方法 采用盐酸溶液将吗啉脂肪酸盐酸解成吗啉, 氢氧化钠溶液调节溶液酸碱度, 气相色谱-氢火焰离子化检测器测定。结果 方法的基质效应为96.67%; 样品空白、试剂空白和标准溶液空白对目标物定性不存在干扰; 不同浓度的样品在48 h内进样峰面积的偏差在±5%以内; 采用本方法对市售实际样品进行分析, 12 批次样品检出吗啉。结论 该方法干扰小、特异性强、重复性好, 前处理简单、绿色, 可为吗啉脂肪酸盐果蜡中吗啉的鉴别提供技术支撑。

, correspAuthors=汪薇, authorNote=null, correspAuthorsNote=
* 汪薇(1989—), 女, 博士, 高级工程师, 主要研究方向为食品安全检测。E-mail:
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李贝贝(1993—), 女, 硕士, 助理工程师, 主要研究方向为食品安全检测。E-mail:

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李贝贝(1993—), 女, 硕士, 助理工程师, 主要研究方向为食品安全检测。E-mail:

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Guangzhou: South China Agricultural University, 2019., articleTitle=null, refAbstract=null)], funds=[Fund(id=1167158639719625128, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, awardId=2018YFC1602303, language=CN, fundingSource=国家重点研发计划项目(2018YFC1602303), fundOrder=null, country=null), Fund(id=1167158639778345387, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, awardId=2023MK086, language=CN, fundingSource=国家市场监督管理总局科技计划项目(2023MK086), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1167158636582285628, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, xref=null, ext=[AuthorCompanyExt(id=1167158636590674237, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, companyId=1167158636582285628, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1. 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Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Wuhan 430075, China), AuthorCompanyExt(id=1167158636812972362, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, companyId=1167158636804583752, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3.湖北省食品质量安全检测工程技术研究中心, 武汉 430075)])], figs=[ArticleFig(id=1167158638687826309, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, language=EN, label=Fig.1, caption=Gas chromatogram, figureFileSmall=vHCmf0aKg8Wjum6Dq09QPg==, figureFileBig=xNL1Lg50/7P+c7Wh2DMvWA==, tableContent=null), ArticleFig(id=1167158638746546567, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, language=CN, label=图1, caption=气相色谱图

注: a. HP-5的吗啉标准溶液图谱; b. DB-624的吗啉标准溶液图谱; c. Volatile Amine的吗啉标准溶液图谱; d. Volatile Amine的吗啉脂肪酸盐样品图谱。

, figureFileSmall=vHCmf0aKg8Wjum6Dq09QPg==, figureFileBig=xNL1Lg50/7P+c7Wh2DMvWA==, tableContent=null), ArticleFig(id=1167158638826238346, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, language=EN, label=Fig.2, caption=Test chromatograms of accuracy and precision, figureFileSmall=6Qlwr2DA/JYbyBr9yF+A0g==, figureFileBig=upQCxAd4fEsGf5l2lzXWiA==, tableContent=null), ArticleFig(id=1167158638901735821, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, language=CN, label=图2, caption=准确度和精密度实验色谱图

注: a. 低浓度样品; b. 高浓度样品; c. 空白样品。

, figureFileSmall=6Qlwr2DA/JYbyBr9yF+A0g==, figureFileBig=upQCxAd4fEsGf5l2lzXWiA==, tableContent=null), ArticleFig(id=1167158638968844688, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, language=EN, label=Fig.3, caption=Test chromatograms of specificity, figureFileSmall=GUwLMBwKYgl/i87hiirYDw==, figureFileBig=0Pt8vvw4wp0rPCkJ8T/sYQ==, tableContent=null), ArticleFig(id=1167158639027564947, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, language=CN, label=图3, caption=特异性实验色谱图

注: a. 样品空白; b. 试剂空白; c. 标准溶液空白。

, figureFileSmall=GUwLMBwKYgl/i87hiirYDw==, figureFileBig=0Pt8vvw4wp0rPCkJ8T/sYQ==, tableContent=null), ArticleFig(id=1167158639107256726, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, language=EN, label=Table 1, caption=

Comparison and application of chromatographic columns

, figureFileSmall=null, figureFileBig=null, tableContent=
色谱柱 色谱柱极性 固定相 应用
HP-5 (30 m×0.32 mm, 0.25 μm) 弱极性 5%苯基-95%二甲基聚硅氧烷 半挥发性化合物、生物碱、药物、脂肪酸甲酯、卤代化合物、农药、除草剂
DB-624 (30 m×0.32 mm, 1.4 μm) 中等极性 6%氰丙基苯基-94%二甲基聚硅氧烷 挥发性有机物、残留溶剂
Volatile Amine (30 m×0.32 mm,
1.0 μm)		 低极性 胺去活的低极性聚硅氧烷 挥发性胺类
), ArticleFig(id=1167158639170171289, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, language=CN, label=表1, caption=

色谱柱的对比及应用

, figureFileSmall=null, figureFileBig=null, tableContent=
色谱柱 色谱柱极性 固定相 应用
HP-5 (30 m×0.32 mm, 0.25 μm) 弱极性 5%苯基-95%二甲基聚硅氧烷 半挥发性化合物、生物碱、药物、脂肪酸甲酯、卤代化合物、农药、除草剂
DB-624 (30 m×0.32 mm, 1.4 μm) 中等极性 6%氰丙基苯基-94%二甲基聚硅氧烷 挥发性有机物、残留溶剂
Volatile Amine (30 m×0.32 mm,
1.0 μm)		 低极性 胺去活的低极性聚硅氧烷 挥发性胺类
), ArticleFig(id=1167158639262445980, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, language=EN, label=Table 2, caption=

Results of method accuracy and precision

, figureFileSmall=null, figureFileBig=null, tableContent=
加标含量水平 1 2 3 4 5
空白 阴性 阴性 阴性 阴性 阴性
低浓度 阳性 阳性 阳性 阳性 阳性
高浓度 阳性 阳性 阳性 阳性 阳性
), ArticleFig(id=1167158639350526367, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, language=CN, label=表2, caption=

方法的准确度和精密度结果

, figureFileSmall=null, figureFileBig=null, tableContent=
加标含量水平 1 2 3 4 5
空白 阴性 阴性 阴性 阴性 阴性
低浓度 阳性 阳性 阳性 阳性 阳性
高浓度 阳性 阳性 阳性 阳性 阳性
), ArticleFig(id=1167158639451189666, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, language=EN, label=Table 3, caption=

Summary of morpholine detected in actual samples

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称 厂家 含量/(g/kg)
吗啉脂肪酸盐果蜡-1 宜昌美亮工贸有限责任公司 19.058±0.180
吗啉脂肪酸盐果蜡-2 宜昌美亮工贸有限责任公司 14.508±0.078
吗啉脂肪酸盐果蜡-3 宜昌美亮工贸有限责任公司 12.714±0.057
吗啉脂肪酸盐果蜡-4 宜昌浏江缘工贸有限公司 29.406±0.100
吗啉脂肪酸盐果蜡-5 宜昌浏江缘工贸有限公司 42.484±0.018
吗啉脂肪酸盐果蜡-6 宜昌浏江缘工贸有限公司 34.008±0.190
吗啉脂肪酸盐果蜡-7 宜昌海杰生物科技有限公司 44.668±0.150
吗啉脂肪酸盐果蜡-8 宜昌海杰生物科技有限公司 34.242±0.160
吗啉脂肪酸盐果蜡-9 宜昌海杰生物科技有限公司 33.696±0.140
吗啉脂肪酸盐果蜡-10 珠海绿色鲜程生物技术公司 13.624±0.024
吗啉脂肪酸盐果蜡-11 珠海绿色鲜程生物技术公司 17.888±0.034
吗啉脂肪酸盐果蜡-12 珠海绿色鲜程生物技术公司 16.354±0.023
), ArticleFig(id=1167158639547658661, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881494868931009, language=CN, label=表3, caption=

实际样品中检出吗啉的情况汇总

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称 厂家 含量/(g/kg)
吗啉脂肪酸盐果蜡-1 宜昌美亮工贸有限责任公司 19.058±0.180
吗啉脂肪酸盐果蜡-2 宜昌美亮工贸有限责任公司 14.508±0.078
吗啉脂肪酸盐果蜡-3 宜昌美亮工贸有限责任公司 12.714±0.057
吗啉脂肪酸盐果蜡-4 宜昌浏江缘工贸有限公司 29.406±0.100
吗啉脂肪酸盐果蜡-5 宜昌浏江缘工贸有限公司 42.484±0.018
吗啉脂肪酸盐果蜡-6 宜昌浏江缘工贸有限公司 34.008±0.190
吗啉脂肪酸盐果蜡-7 宜昌海杰生物科技有限公司 44.668±0.150
吗啉脂肪酸盐果蜡-8 宜昌海杰生物科技有限公司 34.242±0.160
吗啉脂肪酸盐果蜡-9 宜昌海杰生物科技有限公司 33.696±0.140
吗啉脂肪酸盐果蜡-10 珠海绿色鲜程生物技术公司 13.624±0.024
吗啉脂肪酸盐果蜡-11 珠海绿色鲜程生物技术公司 17.888±0.034
吗啉脂肪酸盐果蜡-12 珠海绿色鲜程生物技术公司 16.354±0.023
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气相色谱法鉴别吗啉脂肪酸盐果蜡中的吗啉
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李贝贝 1, 2, 3 , 张菊 1, 2, 3 , 汪薇 1, 2, 3, *
食品安全质量检测学报 | 专题：食品中有毒有害物质分析与监测 2025,16(10): 173-178
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食品安全质量检测学报 | 专题：食品中有毒有害物质分析与监测 2025, 16(10): 173-178
气相色谱法鉴别吗啉脂肪酸盐果蜡中的吗啉
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李贝贝1, 2, 3 , 张菊1, 2, 3, 汪薇1, 2, 3, *
作者信息
  • 1.湖北省食品质量安全监督检验研究院, 武汉 430075
  • 2.国家市场监督管理总局重点实验室(动物源性食品中重点化学危害物检测技术), 武汉 430075
  • 3.湖北省食品质量安全检测工程技术研究中心, 武汉 430075

    • 李贝贝(1993—), 女, 硕士, 助理工程师, 主要研究方向为食品安全检测。E-mail:

通讯作者:

* 汪薇(1989—), 女, 博士, 高级工程师, 主要研究方向为食品安全检测。E-mail:
Identification of morpholine in morpholine fatty acid salt fruit wax by gas chromatography
Bei-Bei LI1, 2, 3 , Ju ZHANG1, 2, 3, Wei WANG1, 2, 3, *
Affiliations
  • 1. Hubei Provincial Institute for Food Supervision and Test, Wuhan 430075, China
  • 2. Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal-derived Food, State Administration for Market Regulation, Wuhan 430075, China
  • 3. Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Wuhan 430075, China
出版时间: 2025-05-25 doi: 10.19812/j.cnki.jfsq11-5956/ts.20241112002
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摘要
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目的 建立气相色谱法鉴别吗啉脂肪酸盐果蜡中的吗啉。方法 采用盐酸溶液将吗啉脂肪酸盐酸解成吗啉, 氢氧化钠溶液调节溶液酸碱度, 气相色谱-氢火焰离子化检测器测定。结果 方法的基质效应为96.67%; 样品空白、试剂空白和标准溶液空白对目标物定性不存在干扰; 不同浓度的样品在48 h内进样峰面积的偏差在±5%以内; 采用本方法对市售实际样品进行分析, 12 批次样品检出吗啉。结论 该方法干扰小、特异性强、重复性好, 前处理简单、绿色, 可为吗啉脂肪酸盐果蜡中吗啉的鉴别提供技术支撑。

吗啉脂肪酸盐果蜡  /  气相色谱法  /  吗啉  /  鉴别

Objective To establish a method for the identification of morpholine in morpholine fatty acid salt fruit wax by gas chromatography. Methods Morpholine fatty acid salt was hydrolyzed to morpholine using hydrochloric acid solution, and the pH of the solution was adjusted with sodium hydroxide acid solution. Detection was performed using gas chromatography-hydrogen flame ionization detector. Results The matrix effect of the method was 96.67%; there was no interference from sample blanks, reagent blanks, and standard solution blanks on the qualitative analysis of the target substance; the deviation of peak area for samples of different concentrations within 48 hours was within ±5%. The method was used to analyze the actual commercial samples, and 12 batches of samples were detected morpholine. Conclusion This method has the advantages of minimal interference, strong specificity, and good repeatability. The pretreatment process is simple and environmentally friendly, providing technical support for the identification of morpholine in morpholine fatty acid salt fruit wax.

morpholine fatty acid salt fruit wax  /  gas chromatography  /  morpholine  /  identification
李贝贝, 张菊, 汪薇. 气相色谱法鉴别吗啉脂肪酸盐果蜡中的吗啉. 食品安全质量检测学报, 2025 , 16 (10) : 173 -178 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241112002
Bei-Bei LI, Ju ZHANG, Wei WANG. Identification of morpholine in morpholine fatty acid salt fruit wax by gas chromatography[J]. Journal of Food Safety & Quality, 2025 , 16 (10) : 173 -178 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241112002
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0 引言
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吗啉脂肪酸盐为黄棕色、棕褐色透明或半透明乳液, 易溶于水和乙醇, 大量溶解于水中时呈凝胶状[1-3]。以吗啉、食用油脂或脂肪酸(辛酸、癸酸、月桂酸、豆蔻酸、棕榈酸、硬脂酸、油酸)和天然动植物蜡(如棕榈蜡)或天然动植物胶(如紫胶、松香)为原料[4-5], 在一定温度下反应制成的食品添加剂吗啉脂肪酸盐果蜡, 作为被膜剂用于经表面处理的鲜水果[6-9]。
人体摄食吗啉脂肪酸盐后在体内分解成吗啉和相应的脂肪酸[10]。对吗啉毒性的动物学研究表明, 特定剂量和时间的吗啉暴露, 会引起肝、肾、胃的损伤[5]。此外, 一定剂量的吗啉与亚硝酸盐类共同摄入, 可能生成N-亚硝基吗啉, N-亚硝基吗啉可引起实验动物发生肝、肾、胃肿瘤[11-14], 具有潜在风险。作为世界水果生产大国, 我国水果保鲜被膜剂的需求量不断攀升, 吗啉作为吗啉脂肪酸盐果蜡中的潜在风险成分, 其安全性引起了消费者的广泛关注和媒体的热议。鉴于此, 国家食品安全风险评估专家委员会对吗啉脂肪酸盐果蜡进行了全面的风险评估[11], 结果表明, 在一般的膳食消费水平下, 通过主要水果及果汁摄入的吗啉水平对我国消费者健康造成的风险处于可接受水平。使用吗啉作为原料的吗啉脂肪酸盐果蜡不会对人体健康构成威胁, 即使考虑通过包装材料、环境等其他途径摄入的吗啉, 其带来的风险也处于可接受范围, 因此, 目前仅对吗啉进行了定性检测分析, 而未构建定量分析方法。
针对吗啉脂肪酸盐果蜡中吗啉的定性分析, 目前主要采用的检测技术包括气相色谱法[15]、液相色谱法、气相色谱-质谱法[17-19]以及液相色谱-质谱法[16,20-22]。这些技术通常依赖于将吗啉通过亚硝基化反应转化成为N-亚硝基吗啉来进行分析。然而, 该分析方法需要额外的化学反应步骤, 增加了实验操作的复杂性和时间消耗, 亚硝基化反应可能不完全, 反应条件也可能影响结果的准确性, 同时还需要额外的试剂和可能的设备, 增加分析成本。基于此, 本研究参考了日本食品添加物公定书(Japanese food additives public regulations, JSFA9)[23], 开发了一种气相色谱鉴别方法, 旨在简化分析流程、减少环境污染、降低分析成本、减少误差的引入, 并为制定相关标准提供参考依据, 为吗啉脂肪酸盐果蜡中吗啉的定性分析提供了一种新的技术途径。
1 材料与方法
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1.1 材料与试剂
吗啉标准品(纯度≥99%, 加拿大Toronto Research Chemicals公司); 盐酸、氢氧化钠(优级纯, 国药集团化学试剂有限公司); 甲醇(色谱纯, 湖北弗顿科学技术有限公司)。
1.2 仪器与设备
7890B型气相色谱仪(配有氢火焰离子化检测器, 美国Agilent公司); DM-Volatile Amine石英毛细管柱(30 m× 0.32 mm, 5 μm)(北京迪科马科技有限公司); Milli-Q去离子水发生器(美国Millipore公司); WH-5恒温水浴装置(杭州佑宁仪器有限公司); XPR105DR电子天平(精度为0.0001 g)、S210-K pH计(梅特勒-托利多仪器上海有限公司)。
1.3 实验方法
1.3.1 标准溶液配制
准确称取0.05 g吗啉标准品(精确至0.0001 g)于100 mL容量瓶中, 用甲醇溶解并定容制成质量浓度为0.5 mg/mL的标准储备液, 混匀, 于−20 ℃下避光保存, 备用。
1.3.2 样品前处理
称取2 g吗啉脂肪酸盐果蜡试样, 加入10 mL盐酸溶液(30 mL盐酸加入50 mL水中), 在60 ℃水浴加热10 min, 冷却至室温, 过滤。取滤液5 mL, 加入1.5 mL氢氧化钠溶液(600 g/L), 使得溶液呈碱性, 取一定量的上述溶液与甲醇按1:3体积比混匀, 供GC测定。
1.3.3 仪器条件
升温程序: 初温50 ℃保持1 min, 30 ℃/min升温至250 ℃保持4 min, 20 ℃/min升温至270 ℃保持2 min; 进样口温度: 200 ℃, 进样方式: 分流模式, 分流比30:1, 恒流模式, 进样量1 μL; 检测器温度: 280 ℃; 载气: 高纯氮气, 流量1.0 mL/min, 氢气: 30 mL/min, 空气: 330 mL/min。
1.3.4 方法学考察
实验室评价基质效应常用的方法有柱后注射法、提取后添加法、相对响应值法、校准曲线测定法等[24-25]。本研究采用相对响应值法评价基质效应。实验中采用甲醇作为溶剂配制质量浓度为0.5 mg/mL的吗啉, 作为溶剂标准溶液; 采用吗啉脂肪酸盐果蜡空白样品基质溶液作为溶剂配制质量浓度为0.5 mg/mL的吗啉, 作为基质标准溶液。采用相同仪器方法于气相色谱仪上进行检测。基质效应计算如公式(1):
$\text { 基质效应 } /\%=\frac{B}{A} \times 100 \%$
式中: A为纯溶剂中标准溶液的响应值; B为样品基质中添加相同含量标准溶液的响应值。
1.4 数据处理
所有实验重复3次测定, 通过Masshunter 10.0软件对实验数据进行分析处理并制图。采用WPS Office 2023和Oringin 2024软件进行数据分析和绘图。
2 结果与分析
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2.1 色谱条件的优化
吗啉属非极性碱性化合物, 吗啉的检测选用的色谱柱固定相类型主要有弱极性的5%苯基-95%二甲基聚硅氧烷、非极性的碱性化合物分析柱、极性的硝基对苯二酸改性的聚乙二醇。本方法对比了3种类型的色谱柱, 分别是弱极性的HP-5型色谱柱、中等极性的DB-624型色谱柱以及低极性的Volatile Amine型色谱柱, 3种色谱柱的固定相、极性和应用范围见表1。
实验表明, HP-5型色谱柱在分离吗啉标准溶液时, 吗啉色谱峰在HP-5型色谱柱上峰型拖尾严重; DB-624型色谱柱分离吗啉标准溶液时, 由于色谱柱固定相为中等极性的聚硅氧烷, 其对非极性化合物的保留能力较弱, 导致峰响应明显低于其他型号的色谱柱, 且峰型拖尾严重; 当用低极性的Volatile Amine型色谱柱分离吗啉标准溶液和吗啉脂肪酸盐果蜡样品时, 吗啉色谱峰和样品峰的拖尾因子T符合《中国药典》规定T在0.95~1.05之间[26], 且在分离样品时无干扰, 故本研究选择了专为挥发性胺类物质分析、表面具有强惰性的Volatile Amine型色谱柱。分离后的气相色谱图如图1。
2.2 前处理条件的优化
吗啉脂肪酸盐果蜡样品中加入盐酸进行酸解, 酸解过程通常是不可逆放热反应, 分解率较高, 释放的热量可使物料温度升高, 温度升高可使大多数物质的溶解度和扩散系数增加, 溶液黏度减小, 酸解速率提高, 因而加快反应速度[27]。考察100、80、60 ℃不同水浴温度对吗啉脂肪酸盐样品酸解的影响, 吗啉在100、80、60 ℃水浴温度下响应基本不变, 40 ℃水浴温度下响应相对较低, 可能是由于在起始温度为40 ℃水解10 min条件下, 样品未完全水解, 考虑节约能耗和保证实验安全的情况下, 故选择水浴温度为60 ℃。
氢氧化钠在100 mL水中的溶解度随温度增加而增大, 当温度为10 ℃时其溶解度是51 g/100 mL, 当温度为20 ℃其溶解度是109 g/100 mL, 基于对外界温度条件和实验安全的考量, 最终选择氢氧化钠质量浓度为60 g/100 mL, 即600 g/L。氢氧化钠溶液的加入体积确定为1.5 mL, 因为加入此体积可使不同类型样品的溶液均呈碱性, 且稀释倍数小, 可保证合适检出限。
2.3 方法学评价
2.3.1 基质效应评价
质量浓度为0.5 mg/mL吗啉溶剂标准溶液色谱峰峰面积为125.9439 pA, 质量浓度为0.5 mg/mL吗啉基质标准溶液色谱峰峰面积为121.7455 pA, 通过公式计算, 得到吗啉在吗啉脂肪酸盐果蜡样品中基质效应为96.67%, 范围在80%~120%之间, 基质效应不明显[28], 在实际检测中采用溶剂标准溶液分析即可。
2.3.2 准确度、精密度和特异性
在方法验证中定性分析的精密度通常表示为假阳性或假阴性率, 其可以用不同的浓度水平来确定[29]。分析了含量水平为空白、低浓度(2.5 g/kg)和高浓度(50 g/kg)的3个含量水平的样品。实验结果如表2, 空白样品结果为阴性, 低高浓度样品结果为阳性, 色谱图见图2, 实验结果与实际数据结果一致。
采用分析一定数量的代表性空白样品, 观察在目标分析物出现的区域色谱出峰情况, 确定是否存在干扰[30]。本研究对样品空白、试剂空白、标准溶液空白进行3平行检测。实验结果对应的色谱图见图3, 结果显示不同空白对目标物保留时间范围内和对目标物定性均不存在干扰。
2.3.3 标准溶液及样液的稳定性
标准溶液的稳定性测试: 配制1 mg/mL的吗啉标准储备液, 冷冻避光保存, 分别放置0、10、20、30、60、90 d进行测定, 每次以新配制的相同浓度标准溶液去标定放置一段时间的标准溶液浓度, 进行稳定性考察。将储存不同时长的标准溶液与同期新配标准溶液的色谱峰响应值相比较, 标准溶液峰面积偏差随时间的变化偏差均控制在±5%内, 这一结果表明, 标准储备液在冷冻避光保存3个月条件下具有良好的稳定性。
试样溶液的稳定性: 准确称取样品2.0 g, 向其中分别准确加入质量浓度为50 mg/mL的吗啉标准溶液0.10、0.5、1.0 mL, 配制低中高3个加标浓度水平的样品, 样品经处理后, 分别于1、3、5、12、24、48 h时间点进样分析, 考察相同含量的样品在放置不同时间进样后峰面积的偏差。结果表明, 不同浓度的样品在48 h之内进样, 其峰面积偏差均控制在±5%以内, 表明试样溶液在该时间范围内具有较好的稳定性。
2.4 实际样品分析
本研究从市场上购买了一些具有代表性的实际样品(共14批次)进行测定。经实验测定表明, 检出含吗啉的样品共12批次, 检测结果如表3所示。结果表明, 在检出的样品中吗啉的保留时间未出现偏移, 吗啉的含量在12.714~44.668 g/kg之间, 能达到鉴别的目的。
3 结论
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本研究建立了一种利用气相色谱法测定吗啉脂肪酸盐果蜡中吗啉含量的新方法。该方法简化了样品前处理流程, 无需过柱或浓缩, 显著降低了操作的复杂性和时间成本。本研究减少了有机溶剂的使用量, 降低了对环境的潜在影响, 且仅需少量样品即可进行准确测定实验。该方法具有干扰少、灵敏度高、重复性好等优点, 能够有效地进行吗啉的鉴别。综上所述, 本研究方法不仅提升了测定效率和准确性, 还为吗啉脂肪酸盐果蜡的鉴别提供了一种有效的技术手段。预期该方法将在食品添加剂检测领域获得广泛应用, 并为相关标准的制定和更新提供科学依据。
基金
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  • 国家重点研发计划项目(2018YFC1602303)
  • 国家市场监督管理总局科技计划项目(2023MK086)
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2025年第16卷第10期
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20241112002
  • 接收时间：2024-11-12
  • 首发时间：2025-07-15
  • 出版时间：2025-05-25
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  • 收稿日期：2024-11-12
基金
国家重点研发计划项目(2018YFC1602303)
国家市场监督管理总局科技计划项目(2023MK086)
作者信息
    1.湖北省食品质量安全监督检验研究院, 武汉 430075
    2.国家市场监督管理总局重点实验室(动物源性食品中重点化学危害物检测技术), 武汉 430075
    3.湖北省食品质量安全检测工程技术研究中心, 武汉 430075

通讯作者:

* 汪薇(1989—), 女, 博士, 高级工程师, 主要研究方向为食品安全检测。E-mail:
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https://castjournals.cast.org.cn/joweb/spaq/CN/10.19812/j.cnki.jfsq11-5956/ts.20241112002
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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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