香精中丙烯酸乙酯、反-2-庚烯醛、苄叉丙酮和对叔丁基苯酚的测定方法研究
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摘要
建立了同时检测香精中丙烯酸乙酯、反-2-庚烯醛、苄叉丙酮和对叔丁基苯酚4种禁用物质的气相色谱-质谱(GC-MS)方法,并对方法进行了验证。结果表明:该方法在0.0005 mg/mL到0.1000 mg/mL的质量浓度范围呈现良好的线性关系,相关系数均大于0.9900;回收率在95%~113%之间,精密度在1.42%~3.94%之间,检出限为0.005μg/mL(S/N≥3),满足痕量分析检测要求,可用于香精中禁用物质丙烯酸乙酯、反-2-庚烯醛、苄叉丙酮和对叔丁基苯酚的定性定量测定。应用该方法分析检测薄荷香精样品中的丙烯酸乙酯、反-2-庚烯醛、苄叉丙酮和对叔丁基苯酚,结果未发现阳性样品。
In this study, a gas chromatography-mass spectrometry(GC-MS) method was established for the simultaneous determination of ethyl acrylate, trans-2-heptenal, benzylidene acetone and p-tert-butylphenol in ?avors, and the method was also validated. The results showed that the method had a good linearity in the concentration range of 0.0005 mg/mL to0.1000 mg/mL, the correlation coefficient was greater than 0.9900. And the recoveries were between 95% and 113% with relative standard deviation(RSD) from 1.42% to 3.94%. The detection limit was 0.005 μg/m L(S/N not less than 3), which met the requirements of trace analytical detection. It can be used to detect the banned ingredients including ethyl acrylate, trans-2-heptenal, benzylidene acetone and p-tert-butylphenol in ?avors. When the method was applied to detect ethyl acrylate, trans-2-heptenal, benzylidene acetone and p-tert-butylphenol in 10 peppermint ?avor samples, no positive sample was found.
In this study, a gas chromatography-mass spectrometry(GC-MS) method was established for the simultaneous determination of ethyl acrylate, trans-2-heptenal, benzylidene acetone and p-tert-butylphenol in ?avors, and the method was also validated. The results showed that the method had a good linearity in the concentration range of 0.0005 mg/mL to0.1000 mg/mL, the correlation coefficient was greater than 0.9900. And the recoveries were between 95% and 113% with relative standard deviation(RSD) from 1.42% to 3.94%. The detection limit was 0.005 μg/m L(S/N not less than 3), which met the requirements of trace analytical detection. It can be used to detect the banned ingredients including ethyl acrylate, trans-2-heptenal, benzylidene acetone and p-tert-butylphenol in ?avors. When the method was applied to detect ethyl acrylate, trans-2-heptenal, benzylidene acetone and p-tert-butylphenol in 10 peppermint ?avor samples, no positive sample was found.
引文
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[12]曾莉,张炤,刘丹,等.气相色谱-质谱法同时测定肉制品中的12种多环芳烃[J].中国卫生检验杂志,2017(17):2486-2488.
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[2]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.香精:GB/T 22731[S].北京:中国标准出版社,2017.
[3]国家食品药品监督管理总局.世界卫生组织国际癌症研究机构致癌物清单[EB/OL].(2017-12-06)[2018-04-03].http://www.ada.gov.cn/wap/public/content/8312718.
[4]化学工业出版社辞书编辑部.化学化工大辞典[M].北京:化学工业出版社,2003.
[5]张明森,主编.精细有机化工中间体全书[M].北京:化学工业出版社,2008.
[6]张皓冰,何昱,贾国惠,等.气相色谱/质谱(GC/MS)联用技术对麝香的多成分含量分析[J].中成药,2002,24(11):868-871.
[7]吴春英,白鹭,陆文龙,等.气相色谱-串联质谱法同时快速检测环境水样中11种合成麝香[J].分析科学学报,2016,32(2):188-192.
[8]QIN Z,PANG X,CHEN D,et al.Evaluation of Chinese tea by the electronic nose and gas chromatography-mass spectrometry:Correlation with sensory properties and classification according to grade level[J].Food Research International,2013,53(2):864-874.
[9]MAYR C M,CAPONE D L,PARDON K H,et al.Quantitative analysis by GC-MS/MS of 18 aroma compounds related to oxidative off-flavor in wines[J].Journal of Agricultural&Food Chemistry,2015,63(13):3394-3401.
[10]金红利.气相色谱-质谱法检测化妆品中防腐剂测定方法的研究[D].大连:大连工业大学,2011.
[11]司晓喜,张凤梅,刘志华,等.气相色谱-负化学电离源-飞行时间质谱筛查和定量测定天然香精中3种农药残留[J].化学试剂,2016,38(12):1191-1195.
[12]曾莉,张炤,刘丹,等.气相色谱-质谱法同时测定肉制品中的12种多环芳烃[J].中国卫生检验杂志,2017(17):2486-2488.
[13]李长于,李祖光,周示玉,等.气相色谱-串联质谱法测定香精香料中的香豆素和黄樟素[J].质谱学报,2011,32(5):265-270.