Article(id=1153433693512257947, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153433686872679135, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20241025009, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1729785600000, receivedDateStr=2024-10-25, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1752929622295, onlineDateStr=2025-07-19, pubDate=1744646400000, pubDateStr=2025-04-15, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1752929622295, onlineIssueDateStr=2025-07-19, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1752929622295, creator=13701087609, updateTime=1752929622295, updator=13701087609, issue=Issue{id=1153433686872679135, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='7', pageStart='1', pageEnd='322', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1752929620712, creator=13701087609, updateTime=1757656380159, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1173259152974561742, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153433686872679135, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1173259152978756047, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153433686872679135, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=248, endPage=254, ext={EN=ArticleExt(id=1153433694355313067, articleId=1153433693512257947, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Determination of 9 kinds of short-chain fatty acids in salt by headspace solid phase microextraction arrow-gas chromatography-mass spectrometry, columnId=1151895321388347923, journalTitle=Journal of Food Safety & Quality, columnName=Food Analysis and Detection, runingTitle=null, highlight=null, articleAbstract=

Objective To establish a qualitative and quantitative analytical method for determination of short-chain fatty acids in table salt using headspace solid phase microextraction arrow-gas chromatography-mass spectrometry. Methods A phosphoric acid solution was added to the salt samples, and the headspace solid phase microextraction arrow technique was employed to extract and enrich the short-chain fatty acids. The effects of extraction fiber, extraction temperature, extraction time, and incubation time on the extraction efficiency were investigated. The target compounds were detected by gas chromatography-mass spectrometry and quantified using the external standard method. Results The 100 μm Polyacrylate extraction fiber demonstrated good selectivity for short-chain fatty acids. Under optimal conditions (extraction temperature of 40 °C, extraction time of 30 min, desorption time of 5 min and incubation time of 20 min), the method showed excellent linearity for 9 kinds of short-chain fatty acids, with correlation coefficients greater than 0.995. The limits of detection ranged from 0.25 to 25.00 μg/kg, the recovery rates were between 92.2% and 100.1%, and the relative standard deviations ranged from 1.4% to 9.4%. Conclusion The established method for analyzing short-chain fatty acids in table salt is characterized by simple sample preparation, high sensitivity, good recovery rates and stability, making it suitable for the detection of short-chain fatty acids in table salt.

, correspAuthors=Xiao-Xiao WU, 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=Jing-Jing XU, Xiao-Xiao WU, Di-Yao JIANG, Chi ZHANG, Lan-Ling CHU, Han-Xu JI), CN=ArticleExt(id=1153433724369752423, articleId=1153433693512257947, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=顶空箭形固相微萃取-气相色谱-质谱法测定食盐中9种短链脂肪酸, columnId=1151895321958773274, journalTitle=食品安全质量检测学报, columnName=食品分析与检测, runingTitle=null, highlight=null, articleAbstract=

目的 建立顶空箭形固相微萃取-气相色谱-质谱法测定食盐中短链脂肪酸的定性和定量分析方法。方法 在食盐样品中加入磷酸溶液, 基于箭形固相微萃取技术对短链脂肪酸进行萃取富集, 探究了萃取头、萃取温度、萃取时间、孵育时间对萃取效果的影响, 目标物用气相色谱-质谱法检测, 外标法定量。结果 萃取头100 μm Polyacrylate对短链脂肪酸有较好的选择性, 在萃取温度40 ℃、时间30 min, 解析时间5 min, 孵育时间20 min的条件下, 9种短链脂肪酸线性关系良好, 相关系数大于0.995, 检出限为0.25~25.00 μg/kg, 回收率为92.2%~100.1%, 相对标准偏差为1.4%~9.4%。结论 本研究建立的食盐中短链脂肪酸的分析方法样品制备简单, 灵敏度高, 回收率和稳定性好, 适用于食盐中短链脂肪酸的检测。

, correspAuthors=吴肖肖, authorNote=null, correspAuthorsNote=
* 吴肖肖(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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徐婧婧(1991—), 女, 硕士, 工程师, 主要研究方向为食品安全检测。E-mail:

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注: 1. 乙酸; 2. 丙酸; 3. 异丁酸; 4. 丁酸; 5. 2-甲基丁酸; 6. 戊酸; 7. 2-甲基戊酸; 8. 4-甲基戊酸; 9. 己酸。

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注: 1. 乙酸; 2. 丙酸; 3. 异丁酸; 4. 丁酸; 5. 2-甲基丁酸; 6. 戊酸; 7. 2-甲基戊酸; 8. 己酸。

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Mass spectrometric parameters for analysis of 9 kinds of SCFAs

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序号 目标化合物 保留时间/min 定量离子(m/z) 定性离子(m/z)
1 乙酸 6.86 43 60, 45
2 丙酸 7.94 73 73, 45
3 异丁酸 8.30 43 73, 41
4 丁酸 9.00 60 73, 41
5 2-甲基丁酸 9.49 74 57, 87
6 戊酸 10.27 60 73, 41
7 2-甲基戊酸 10.57 74 87, 43
8 4-甲基戊酸 10.97 57 74, 73
9 己酸 11.43 60 73, 87
), ArticleFig(id=1173311056916132411, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433693512257947, language=CN, label=表1, caption=

9种SCFAs的质谱参数

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序号 目标化合物 保留时间/min 定量离子(m/z) 定性离子(m/z)
1 乙酸 6.86 43 60, 45
2 丙酸 7.94 73 73, 45
3 异丁酸 8.30 43 73, 41
4 丁酸 9.00 60 73, 41
5 2-甲基丁酸 9.49 74 57, 87
6 戊酸 10.27 60 73, 41
7 2-甲基戊酸 10.57 74 87, 43
8 4-甲基戊酸 10.97 57 74, 73
9 己酸 11.43 60 73, 87
), ArticleFig(id=1173311057016795708, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433693512257947, language=EN, label=Table 2, caption=

Regression equations, correlation coefficients, linear ranges and limits of detection of the target compounds

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目标
化合物
线性方程 相关系数
(r)
线性范围
/(μg/kg)
检出限
/(μg/kg)
乙酸 Y=799.01X+50.77 0.9995 125.00~2500.00 25.00
丙酸 Y=2407.83X+98.17 0.9990 12.50~1250.00 2.50
异丁酸 Y=5268.73X+305.26 0.9960 12.50~1250.00 1.25
己酸 Y=20016.92X+468.88 0.9970 2.50~250.00 0.50
丁酸 Y=14003.28X+123.57 0.9990 6.25~250.00 1.25
2-甲基丁酸 Y=18927.86X+223.17 0.9985 2.50~250.00 0.25
4-甲基戊酸 Y=9152.82X+73.45 0.9980 2.50~250.00 0.50
2-甲基戊酸 Y=26180.56X+299.42 0.9951 2.50~250.00 0.25
戊酸 Y=3218.61X+63.50 0.9995 12.50~250.00 2.50
), ArticleFig(id=1173311057113264701, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433693512257947, language=CN, label=表2, caption=

目标化合物的线性方程、相关系数、线性范围和检出限

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目标
化合物
线性方程 相关系数
(r)
线性范围
/(μg/kg)
检出限
/(μg/kg)
乙酸 Y=799.01X+50.77 0.9995 125.00~2500.00 25.00
丙酸 Y=2407.83X+98.17 0.9990 12.50~1250.00 2.50
异丁酸 Y=5268.73X+305.26 0.9960 12.50~1250.00 1.25
己酸 Y=20016.92X+468.88 0.9970 2.50~250.00 0.50
丁酸 Y=14003.28X+123.57 0.9990 6.25~250.00 1.25
2-甲基丁酸 Y=18927.86X+223.17 0.9985 2.50~250.00 0.25
4-甲基戊酸 Y=9152.82X+73.45 0.9980 2.50~250.00 0.50
2-甲基戊酸 Y=26180.56X+299.42 0.9951 2.50~250.00 0.25
戊酸 Y=3218.61X+63.50 0.9995 12.50~250.00 2.50
), ArticleFig(id=1173311057188762174, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433693512257947, language=EN, label=Table 3, caption=

Results of recoveries and precision (n=6)

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目标化合物 加标量/(μg/kg) 回收率/% RSDs/%
乙酸 50 96.3 5.7
250 98.4 1.6
1250 99.3 2.5
丙酸 25 95.6 6.6
125 97.9 3.2
625 97.9 2.7
异丁酸 25 94.7 8.2
125 97.9 4.2
625 100.1 1.4
丁酸 25 96.8 4.1
75 97.5 4.0
125 100.0 4.4
2-甲基丁酸 5 97.4 7.4
25 96.0 6.4
125 99.7 4.4
戊酸 25 98.7 9.2
75 97.1 6.2
125 98.5 4.3
2-甲基戊酸 5 95.5 9.2
25 93.5 9.0
125 96.4 4.4
4-甲基戊酸 5 94.2 5.6
25 94.6 6.1
125 95.2 5.4
己酸 5 92.5 9.4
25 92.2 7.0
125 95.2 5.8
), ArticleFig(id=1173311057264259647, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153433693512257947, language=CN, label=表3, caption=

加标回收率及精密度结果(n=6)

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目标化合物 加标量/(μg/kg) 回收率/% RSDs/%
乙酸 50 96.3 5.7
250 98.4 1.6
1250 99.3 2.5
丙酸 25 95.6 6.6
125 97.9 3.2
625 97.9 2.7
异丁酸 25 94.7 8.2
125 97.9 4.2
625 100.1 1.4
丁酸 25 96.8 4.1
75 97.5 4.0
125 100.0 4.4
2-甲基丁酸 5 97.4 7.4
25 96.0 6.4
125 99.7 4.4
戊酸 25 98.7 9.2
75 97.1 6.2
125 98.5 4.3
2-甲基戊酸 5 95.5 9.2
25 93.5 9.0
125 96.4 4.4
4-甲基戊酸 5 94.2 5.6
25 94.6 6.1
125 95.2 5.4
己酸 5 92.5 9.4
25 92.2 7.0
125 95.2 5.8
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顶空箭形固相微萃取-气相色谱-质谱法测定食盐中9种短链脂肪酸
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徐婧婧 1 , 吴肖肖 1, * , 蒋迪尧 1 , 张驰 1 , 褚兰玲 2 , 纪晗旭 1
食品安全质量检测学报 | 食品分析与检测 2025,16(7): 248-254
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食品安全质量检测学报 | 食品分析与检测 2025, 16(7): 248-254
顶空箭形固相微萃取-气相色谱-质谱法测定食盐中9种短链脂肪酸
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徐婧婧1 , 吴肖肖1, * , 蒋迪尧1, 张驰1, 褚兰玲2, 纪晗旭1
作者信息
  • 1.南京市产品质量监督检验院(南京市质量发展与先进技术应用研究院), 国家市场监督管理总局重点实验室(生物毒素分析与评价), 南京 210019
  • 2.南京林业大学轻工与食品学院, 南京 210037
  • 徐婧婧(1991—), 女, 硕士, 工程师, 主要研究方向为食品安全检测。E-mail:

通讯作者:

* 吴肖肖(1989—), 女, 博士, 高级工程师, 主要研究方向为食品安全检测。E-mail:
Determination of 9 kinds of short-chain fatty acids in salt by headspace solid phase microextraction arrow-gas chromatography-mass spectrometry
Jing-Jing XU1 , Xiao-Xiao WU1, * , Di-Yao JIANG1, Chi ZHANG1, Lan-Ling CHU2, Han-Xu JI1
Affiliations
  • 1. Key Laboratory of Biotoxin Analysis & Assessment, State Administration for Market Regulation, Nanjing Institute of Product Quality Inspection (Nanjing Institute of Quality Development and Advanced Technology Application), Nanjing 210019, China
  • 2. College of Light Industry and Food, Nanjing Forestry University, Nanjing 210037, China
出版时间: 2025-04-15 doi: 10.19812/j.cnki.jfsq11-5956/ts.20241025009
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目的 建立顶空箭形固相微萃取-气相色谱-质谱法测定食盐中短链脂肪酸的定性和定量分析方法。方法 在食盐样品中加入磷酸溶液, 基于箭形固相微萃取技术对短链脂肪酸进行萃取富集, 探究了萃取头、萃取温度、萃取时间、孵育时间对萃取效果的影响, 目标物用气相色谱-质谱法检测, 外标法定量。结果 萃取头100 μm Polyacrylate对短链脂肪酸有较好的选择性, 在萃取温度40 ℃、时间30 min, 解析时间5 min, 孵育时间20 min的条件下, 9种短链脂肪酸线性关系良好, 相关系数大于0.995, 检出限为0.25~25.00 μg/kg, 回收率为92.2%~100.1%, 相对标准偏差为1.4%~9.4%。结论 本研究建立的食盐中短链脂肪酸的分析方法样品制备简单, 灵敏度高, 回收率和稳定性好, 适用于食盐中短链脂肪酸的检测。

食盐  /  短链脂肪酸  /  顶空固相微萃取  /  气相色谱-质谱法

Objective To establish a qualitative and quantitative analytical method for determination of short-chain fatty acids in table salt using headspace solid phase microextraction arrow-gas chromatography-mass spectrometry. Methods A phosphoric acid solution was added to the salt samples, and the headspace solid phase microextraction arrow technique was employed to extract and enrich the short-chain fatty acids. The effects of extraction fiber, extraction temperature, extraction time, and incubation time on the extraction efficiency were investigated. The target compounds were detected by gas chromatography-mass spectrometry and quantified using the external standard method. Results The 100 μm Polyacrylate extraction fiber demonstrated good selectivity for short-chain fatty acids. Under optimal conditions (extraction temperature of 40 °C, extraction time of 30 min, desorption time of 5 min and incubation time of 20 min), the method showed excellent linearity for 9 kinds of short-chain fatty acids, with correlation coefficients greater than 0.995. The limits of detection ranged from 0.25 to 25.00 μg/kg, the recovery rates were between 92.2% and 100.1%, and the relative standard deviations ranged from 1.4% to 9.4%. Conclusion The established method for analyzing short-chain fatty acids in table salt is characterized by simple sample preparation, high sensitivity, good recovery rates and stability, making it suitable for the detection of short-chain fatty acids in table salt.

salt  /  short-chain fatty acids  /  headspace solid phase microextraction  /  gas chromatography-mass spectrometry
徐婧婧, 吴肖肖, 蒋迪尧, 张驰, 褚兰玲, 纪晗旭. 顶空箭形固相微萃取-气相色谱-质谱法测定食盐中9种短链脂肪酸. 食品安全质量检测学报, 2025 , 16 (7) : 248 -254 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241025009
Jing-Jing XU, Xiao-Xiao WU, Di-Yao JIANG, Chi ZHANG, Lan-Ling CHU, Han-Xu JI. Determination of 9 kinds of short-chain fatty acids in salt by headspace solid phase microextraction arrow-gas chromatography-mass spectrometry[J]. Journal of Food Safety & Quality, 2025 , 16 (7) : 248 -254 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241025009
食盐是日常生活的必需品, 是无可替代的调味品[1-3]。随着生活水平的提高, 人们对食盐的要求也越来越高。食盐的质量安全问题不仅关系着人民群众的身体健康和生命安全, 更关系着经济发展和社会稳定[4-7]。2017年, 全国多个省市发现了部分市售的食盐在加热或用手搓后会散发出浓烈的类似于脚臭味的异味[8], 称为“臭脚盐”, 此类产品不符合GB 2721—2015《食品安全国家标准 食用盐》中感官指标要求[9]。研究显示[10], 盐岩沉积及成岩时期, 盐湖中的有机物经氧化分解、还原合成、成岩改造等过程, 使得盐矿中残留部分有机物质, 在食盐生产过程中若除臭工艺不当, 可导致精制盐产品有明显异臭味。冯峰等[11]、张静等[12]在“臭脚盐”中检出了挥发性异味物质主要为丙酸、丁酸、异戊酸等短链脂肪酸(short-chain fatty acids, SCFAs), 并认为SCFAs是导致异味的主要原因。
有研究报道SCFAs与精神分裂症、自闭症等病症密切相关[13-16]。WANG等[17]研究发现自闭症儿童粪便中SCFAs总量显著高于对照组, 李慧慧[18]研究表明首发精神分裂症患者粪便中SCFAs总量、乙酸、异戊酸和已酸含量高于健康对照。而食盐作为不可或缺的调味品, 建立前处理简单、高灵敏、精准的食盐中SCFAs检测方法很有必要。
目前, 食盐中SCFAs的检测方法主要有顶空-气相色谱-质谱法、超高效液相色谱-串联高分辨质谱法等, 现有方法主要聚焦食盐中SCFAs的定性分析, 少数论文中报道的定量方法检测灵敏度不足, 无法满足食盐中SCFAs的痕量、精准检测。顶空固相微萃取技术(solid phase microextraction, SPME)是一种集净化、富集、浓缩于一体的样品分析制备技术[19-24], 箭形固相微萃取与常规的固相微萃取技术相比, 萃取表面积更大、速度更快, 与气相色谱-质谱法联用, 有操作简便, 快速, 灵敏度高, 无溶剂等优势, 已广泛应用于食品中痕量挥发性与半挥发性化合物的提取[25-30]。鉴于此, 本研究将顶空箭形固相微萃取技术与气相色谱-质谱法联用, 对萃取条件进行了优化, 建立了顶空箭形固相微萃取-气相色谱质谱检测食用盐中SCFAs的方法, 可用于异味盐样品的快速区分和食盐中SCFAs的精准检测。
食盐对照样品购买于本地超市, 种类包括: 井矿盐、湖盐、海盐、竹盐, 异味盐, 均为市场委托样品。
乙酸标准品(纯度≥99.9%)、丙酸(纯度≥99.9%)、异丁酸(纯度≥99.8%)、丁酸(纯度≥99.7%)、2-甲基丁酸(纯度≥99.7%)、戊酸(纯度≥99.0%)、2-甲基戊酸(纯度≥98.0%)、4-甲基戊酸(纯度≥99.0%)、己酸(纯度≥99.5%)(上海安谱璀世标准技术服务有限公司); 磷酸、氯化钠(分析纯, 国药集团化学试剂有限公司); 超纯水(Milli-Q超纯水仪制备的超纯水)。
Agilent 8890-5977B气相色谱-质谱联用仪、HP-INNOWAX毛细管色谱柱(30 m×0.32 mm, 0.25 μm, 美国安捷伦公司); Milli-Q IQ7000超纯水系统(德国默克公司); ML304T电子天平[精度为0.1 mg, 梅特勒-托利多仪器(上海)有限公司]; MCA225S-2CCN-I电子天平(精度为0.01 mg, 德国赛多利斯公司)。
称取4 g食盐样品于20 mL顶空样品瓶中, 取0.2% (V:V) 磷酸溶液50 μL加入样品瓶中, 旋紧瓶盖, 涡旋混匀, 待上仪器萃取检测。
准确称取SCFAs标准品, 用超纯水溶解、定容, 配制成9个单标溶液。分别取适量体积的单标溶液, 用超纯水稀释得到混合标准储备液, 其中乙酸质量浓度为5.0 mg/mL, 丙酸、异丁酸质量浓度为2.5 mg/mL, 丁酸、2-甲基丁酸、戊酸、2-甲基戊酸、4-甲基戊酸和己酸的质量浓度为0.5 mg/mL。实验前, 用超纯水将混合标准储备液梯度4~2000倍, 配制成系列浓度混合标准溶液。
用100 μm Polyacrylate箭形固相微萃取头进行萃取, 样品孵育温度为40 ℃, 搅拌速度为1000 r/min, 孵育时间为20 min, 萃取温度为40 ℃, 萃取时间为30 min, 解析时间为5 min。
色谱柱为Agilent HP-INNOWAX (30 m×0.32 mm, 0.25 μm); 载气为氦气(纯度为99.999%), 流速为1.0 mL/min, 不分流模式进样, 进样口温度为250 ℃, 传输线温度为280 ℃; 升温程序: 初始温度60 ℃保持2 min, 以10 ℃/min升至200 ℃保持5 min, 再以10 ℃/min升温至250 ℃, 保持2 min。
质谱条件: 电子轰击离子源, 离子源温度230 ℃, 电子能量70 eV, 四极杆温度150 ℃, 选择离子扫描(selective ion scanning, SIM), 溶剂延迟5 min, 选择离子参数如表1所示。
本研究检测数据的定性定量分析和目标物质色谱图在安捷伦MassHunter软件中完成, 加标回收率和精密度实验重复6次, 其他实验重复3次。采用Excel 2021进行统计计算和绘制图形。
萃取头表面的固定相和涂层厚度影响其对目标物的萃取能力和选择性[31], 固定相的分子结构、官能团、极性等特性决定了萃取头对目标化合物的萃取能力, 根据目标物极性、关键基团、沸点和分配系数等特征参数, 选择合适的萃取头, 可以提高方法的灵敏度和选择性。本研究考察了100 μm Polyacrylate、100 μm PDMS、120 μm Carbon WR/PDMS、120 μm DVB/PDMS、120 μm DVB/Carbon WR/PDMS等5类萃取头对9种SCFAs的选择性和萃取效果。如图1所示, 在相同的色谱质谱条件下, 萃取头100 μm Polyacrylate对各目标物均有较好的萃取效果, 尤其乙酸、丙酸、丁酸和异丁酸。这是因为100 μm Polyacrylate是极性涂层, 对SCFAs等极性物质吸附非常有效。因此, 选择100 μm Polyacrylate萃取头对9种SCFAs进行萃取。
萃取温度影响待测物在气相和液相之间的平衡速度及萃取涂层和气相空间的分配系数。在未平衡状态下, 提高萃取温度, 可加快目标化合物从液体释放至顶空瓶中, 提高萃取效率。但体系温度过高, 也会导致目标化合物从萃取涂层上解吸。本研究考察了35、40、45、50、55、60 ℃等不同温度下, 萃取头100 μm Polyacrylate对SCFAs萃取效率的影响。结果如图2所示, 当温度从35 ℃升高至40 ℃时, 除2-甲基戊酸萃取效率略微降低外, 其他SCFAs的萃取效率都有明显增加或基本保持一致。当温度从40 ℃持续升高时, 大部分目标物萃取效率下降, 尤其是2-甲基戊酸、异丁酸、己酸和2-甲基丁酸萃取效率明显降低。综合考虑, 本研究萃取体系温度选择40 ℃。
在萃取体系未平衡状态下, 延长萃取时间目标物在萃取涂层上的吸附量也会随之增加。本研究考察了在40 ℃萃取温度下, 萃取头100 μm Polyacrylate萃取5、10、15、20、25、30、35、40 min后对SCFAs萃取效率的影响。结果如图3所示, 随着萃取时间增加, SCFAs的峰面积也明显升高。当萃取时间达到30 min, 除乙酸、丙酸、异丁酸外, 其他6个目标物的峰面积基本趋于平稳, 当萃取时间达到40 min, 部分目标物峰面积略微下降。综合萃取效率和检测时长两个因素, 本研究的萃取时间选择30 min。
样品在萃取前先进行加热孵育, 有利于样品中的目标物尽可能释放至顶空瓶中, 提高萃取效率。本研究考察了10、15、20、25、30、35、40 min等不同孵育时间对目标物提取效率的影响。结果如图4所示, 由于大部分目标物萃取效率受孵育时间影响较小, 而2-甲基戊酸和己酸在20 min前峰面积缓慢增加, 在20 min后明显呈下降趋势。因此, 本研究的孵育时间选择20 min。
通过在氯化钠中加入不同浓度的系列SCFAs混合标准溶液, 在优化好的萃取条件下, 按照1.3实验方法进行分析, 9种SCFAs色谱图见图5。以SCFAs的浓度为横坐标, 目标化合物的峰面积为纵坐标, 绘制标准曲线, 目标物化合物的线性方程、相关系数(r)、线性范围见表2。采用标准添加法, 在氯化钠中添加混合标准溶液, 加标浓度逐级递减, 按照“1.3实验方法”进行检测, 以3倍信噪比(signal-to-noise ratio, S/N≥3)计算检出限(limit of detection, LOD)。结果显示, SCFAs在对应的浓度范围内线性良好, 相关系数大于0.995, LODs为0.25~25.00 μg/kg, 满足实验要求。
在空白食盐样品中加入低、中、高3个浓度水平的SCFAs混合标准溶液, 进行加标回收实验, 每个加标水平平行制备6份样品, 按照1.3实验方法进行分析。计算加标回收率和相对标准偏差(relative standard deviation, RSD)。结果见表3, 9种SCFAs的加标回收率为92.2%~100.1%, RSDs为1.4%~9.4%, 精密度与准确度良好。
应用本研究建立的分析方法, 对从本地超市采购的25批次食盐样品以及市场委托的2批次异味盐样品中的9种SCFAs进行检测。结果显示, 2批次异味盐样品中除4-甲基戊酸外, 其他8种SCFAs均有检出, 代表性异味盐样品检测谱图见图6, 其中乙酸含量大于2.0 mg/kg, 丙酸和戊酸含量大于0.1 mg/kg。由于方法灵敏度高, 在少数对照样品中也有微量目标物检出, 如乙酸、丁酸和己酸, 但是含量明显低于异味盐样品。
本研究建立了顶空箭形固相微萃取-气相色谱-质谱法检测食盐中9种SCFAs的方法, 优化了固相微萃取条件。SCFAs在一定的浓度范围内线性良好, 相关系数大于0.995, 方法检出限为0.25~25.00 μg/kg, 加标回收率为92.2%~100.1%, 相对标准偏差为1.4%~9.4%。在实际样品检测中发现异味盐中检出了8种SCFAs, 且乙酸含量较高。该方法操作简单, 灵敏度高, 可用于食盐中SCFAs的精准检测, 具有一定的应用价值和应用前景。
  • 国家重点研发计划项目(2023YFF1105102)
  • 国家市场监管总局科技项目(2022MK160)
  • 江苏省科协青年科技人才托举工程项目(JSTJ-2023-XH007)
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2025年第16卷第7期
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20241025009
  • 接收时间:2024-10-25
  • 首发时间:2025-07-19
  • 出版时间:2025-04-15
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  • 收稿日期:2024-10-25
基金
国家重点研发计划项目(2023YFF1105102)
国家市场监管总局科技项目(2022MK160)
江苏省科协青年科技人才托举工程项目(JSTJ-2023-XH007)
作者信息
    1.南京市产品质量监督检验院(南京市质量发展与先进技术应用研究院), 国家市场监督管理总局重点实验室(生物毒素分析与评价), 南京 210019
    2.南京林业大学轻工与食品学院, 南京 210037

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* 吴肖肖(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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2种不同金属材料的力学参数

Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
total species (%)

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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