QuEChERS前处理结合高效液相色谱-串联质谱法同时测定酵母产品中4种抗氧化剂和5种防腐剂
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摘要
建立高效液相色谱-串联质谱法(high performance liquid chromato graphy-tanelem mass spectrometry,HPLC-MS/MS)法同时测定酵母产品中4种抗氧化剂和5种对羟基苯甲酸酯类防腐剂的定性定量分析方法。样品经溶解脱脂,用正己烷饱和的乙腈提取,浓缩至干流动相复溶,经C_(18)净化、过膜后供仪器测试。采用电喷雾离子源、多重反应监测模式检测,以保留时间和特征离子对比较定性定量。9种分析物在0. 1～10 mg/L相关系数(r~2)均大于0. 992,方法定量限为0. 10～0. 50 mg/kg,酵母产品中3水平6平行的加标回收实验,回收率在78. 9%～108. 6%,相对标准偏差为4. 2%～15. 8%。该方法快速简便、准确可靠,适用于酵母产品中4种抗氧化剂和5种对羟基苯甲酸酯类防腐剂的测定,为高通量检测此类物质提供了技术支持。
A qualitative and quantitative method based on high performance liquid chromatography-tandem mass spectrometry for simultaneous determination of four antioxidants and five p-hydroxybenzoate antiseptics in yeast products was developed. Samples were defatted and extracted with acetonitrile-hexane mixture,and then concentrated to dry and redissolved in the mobile phase. The solution was cleaned by C_(18) powder adsorption and filtered. There were nine analytes determined by using electrospray ion source in multiple reaction monitoring mode. The results showed that all analytes had good linearity in the range of 0. 1-10 mg/L with correlation coefficients(r~2) larger than 0. 992,and the quantitation limits of the method were in the range of 0. 10-0. 50 mg/kg,and the average recovery rate was78. 9%-108. 6%,and RSDs were 4. 2%-15. 8%. This convenient and accurate method provides technical supports for detecting such substances based on high throughput technology.
A qualitative and quantitative method based on high performance liquid chromatography-tandem mass spectrometry for simultaneous determination of four antioxidants and five p-hydroxybenzoate antiseptics in yeast products was developed. Samples were defatted and extracted with acetonitrile-hexane mixture,and then concentrated to dry and redissolved in the mobile phase. The solution was cleaned by C_(18) powder adsorption and filtered. There were nine analytes determined by using electrospray ion source in multiple reaction monitoring mode. The results showed that all analytes had good linearity in the range of 0. 1-10 mg/L with correlation coefficients(r~2) larger than 0. 992,and the quantitation limits of the method were in the range of 0. 10-0. 50 mg/kg,and the average recovery rate was78. 9%-108. 6%,and RSDs were 4. 2%-15. 8%. This convenient and accurate method provides technical supports for detecting such substances based on high throughput technology.
引文
[1]刘绪斌,武运,孟茹.酵母生产技术及安全性检测分析[M].北京:中国质检出版社,2014.
[2]于景芝.酵母生产与应用手册[M].北京:中国轻工业出版社,2005.
[3]罗傲霜,淳泽,罗傲雪,等.食品防腐剂的概况与发展[J].中国食品添加剂,2005,(4):55-58;76.
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[5]林忠洋,马万里,齐迹,等.对羟基苯甲酸酯类防腐剂的人体暴露[J].化学进展,2015,27(5):614-622.
[6]吴晓红.极谱法在食品检测中的应用进展[J].食品安全导刊,2016(33):76-77.
[7]KAMARVDDIN A F,SANABI M M,WAN-IBRAHIM WA,et al.Polypyrrole-magnetite dispersive micro-solidphase extraction combined with ultraviolet-visible spectrophotometry for the determination of rhodamine 6G and crystal violet in textile wastewater[J].Journal of Separation Science,2017,40(21):4 256-4 263.
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[9]CHIANG H C,TSENG R G.Polyamide-kieselguhr thinlayer chromatography of antioxidants[J].Journal of Pharmaceutical Sciences,2010,58(12):1 552-1 553.
[10]李静,王雨,梁立娜.离子色谱法同时测定食品中3种甜味剂和2种防腐剂[J].食品科学,2011,32(12):239-242.
[11]曹小妹,薛江超,高文惠,等.高效毛细管电泳法同时检测饲料中七种防腐剂[J].饲料工业,2012,33(15):61-64.
[12]GARCIA-JIMENEZ J F,VALENCIA M C,CAPITAN-VALLVEY L F.Simultaneous determination of antioxidants,preservatives and sweetener additives in food and cosmetics by flow injection analysis coupled to a monolithic column[J].Analytica Chimica Acta,2007,594(2):226-233.
[13]张社,杨惠琴,唐毅锋,等.比值导数波谱法分析食品中抗氧化剂[J].理化检验(化学分册),2004,40(1):33-34;36.
[14]李艳美,粟有志,李芳,等.Qu ECh ERS前处理高效液相色谱法同时测定酵母产品中7种合成酚类抗氧化剂[J].食品与发酵工业,2017,43(5):198-202.
[15]吴丽容.UPLC法测定食品中多种色素、抗氧化剂、防腐剂和甜味剂[D].厦门:集美大学,2016.
[16]林泽鹏,林晨,王李平,等.毛细管柱气相色谱法对果蔬汁和调味料中脱氢乙酸及4种对羟基苯甲酸酯的测定[J].食品研究与开发,2018,39(14):144-147.
[17]何浩,陈幸莺,梁林富,等.分散液液微萃取-气相色谱法测定复杂食品基质中对羟基苯甲酸酯类[J].食品研究与开发,2017,38(23):146-150.
[18]向俊,漆爱明,毛丽秋.中空纤维膜液相微萃取技术/气相色谱-质谱法对食品中防腐剂与抗氧化剂的测定[J].分析测试学报,2009,28(5):560-563.
[19]李东刚,李春娟,刘敬东.GC-MS-SIM检测糕点中的防腐剂和抗氧化剂[J].分析仪器,2009(4):56-60.
[20]韩熠,刘欣丽,贾晓宇,等.分散液液微萃取-气相色谱-质谱联用法测定饮料中4种对羟基苯甲酸酯类防腐剂[J].分析化学,2009,37(s1):151-151.
[21]张勋,刘韬,吴连鹏,等.高效液相色谱-串联质谱法测定多种食品中7种酚类抗氧化剂和对羟基苯甲酸酯类防腐剂[J].食品与发酵工业,2016,42(11):206-211.
[22]宗珊盈,李超,张娟,等.超高效液相色谱-串联质谱法同时测定食品中7种防腐剂和4种甜味剂[J].中国食品添加剂,2016(6):195-199.
[23]张璐,孔祥虹,李建华,等.固相萃取-超高效液相色谱-电喷雾串联质谱法同时测定食品中13种抗氧化剂[J].分析试验室,2014,33(1):43-47.
[24]HE Z,WANG L,PENG Y,et al.Multiresidue analysis of over 200 pesticides in cereals using a Qu ECh ERS and gas chromatography-tandem mass spectrometry-based method[J].Food Chemistry,2015,169:372-380.
[25]JIA W,LING Y,LIN Y,et al.Analysis of additives in dairy products by liquid chromatography coupled to quadrupole-orbitrap mass spectrometry[J].J Chromatogr A,2014,1 336(7):67-75.
[26]粟有志,马晓雯,孟茹,等.Qu ECh ERS-高效液相色谱-串联质谱法测定酵母抽提物中9种黄色合成色素[J].分析科学学报,2016,32(2):234-238.
[2]于景芝.酵母生产与应用手册[M].北京:中国轻工业出版社,2005.
[3]罗傲霜,淳泽,罗傲雪,等.食品防腐剂的概况与发展[J].中国食品添加剂,2005,(4):55-58;76.
[4]MANI-LOPEZ E,PALOU E,LOPEZ-MALO A.Preservatives:Classifications and analysis[J].Encyclopedia of Food and Health,2016:497-504.
[5]林忠洋,马万里,齐迹,等.对羟基苯甲酸酯类防腐剂的人体暴露[J].化学进展,2015,27(5):614-622.
[6]吴晓红.极谱法在食品检测中的应用进展[J].食品安全导刊,2016(33):76-77.
[7]KAMARVDDIN A F,SANABI M M,WAN-IBRAHIM WA,et al.Polypyrrole-magnetite dispersive micro-solidphase extraction combined with ultraviolet-visible spectrophotometry for the determination of rhodamine 6G and crystal violet in textile wastewater[J].Journal of Separation Science,2017,40(21):4 256-4 263.
[8]DING X J,XIE N,ZHAO S,et al.Simultaneous determination of ten preservatives in ten kinds of foods by micellar electrokinetic chromatography[J].Food Chemistry,2015,181:207-214.
[9]CHIANG H C,TSENG R G.Polyamide-kieselguhr thinlayer chromatography of antioxidants[J].Journal of Pharmaceutical Sciences,2010,58(12):1 552-1 553.
[10]李静,王雨,梁立娜.离子色谱法同时测定食品中3种甜味剂和2种防腐剂[J].食品科学,2011,32(12):239-242.
[11]曹小妹,薛江超,高文惠,等.高效毛细管电泳法同时检测饲料中七种防腐剂[J].饲料工业,2012,33(15):61-64.
[12]GARCIA-JIMENEZ J F,VALENCIA M C,CAPITAN-VALLVEY L F.Simultaneous determination of antioxidants,preservatives and sweetener additives in food and cosmetics by flow injection analysis coupled to a monolithic column[J].Analytica Chimica Acta,2007,594(2):226-233.
[13]张社,杨惠琴,唐毅锋,等.比值导数波谱法分析食品中抗氧化剂[J].理化检验(化学分册),2004,40(1):33-34;36.
[14]李艳美,粟有志,李芳,等.Qu ECh ERS前处理高效液相色谱法同时测定酵母产品中7种合成酚类抗氧化剂[J].食品与发酵工业,2017,43(5):198-202.
[15]吴丽容.UPLC法测定食品中多种色素、抗氧化剂、防腐剂和甜味剂[D].厦门:集美大学,2016.
[16]林泽鹏,林晨,王李平,等.毛细管柱气相色谱法对果蔬汁和调味料中脱氢乙酸及4种对羟基苯甲酸酯的测定[J].食品研究与开发,2018,39(14):144-147.
[17]何浩,陈幸莺,梁林富,等.分散液液微萃取-气相色谱法测定复杂食品基质中对羟基苯甲酸酯类[J].食品研究与开发,2017,38(23):146-150.
[18]向俊,漆爱明,毛丽秋.中空纤维膜液相微萃取技术/气相色谱-质谱法对食品中防腐剂与抗氧化剂的测定[J].分析测试学报,2009,28(5):560-563.
[19]李东刚,李春娟,刘敬东.GC-MS-SIM检测糕点中的防腐剂和抗氧化剂[J].分析仪器,2009(4):56-60.
[20]韩熠,刘欣丽,贾晓宇,等.分散液液微萃取-气相色谱-质谱联用法测定饮料中4种对羟基苯甲酸酯类防腐剂[J].分析化学,2009,37(s1):151-151.
[21]张勋,刘韬,吴连鹏,等.高效液相色谱-串联质谱法测定多种食品中7种酚类抗氧化剂和对羟基苯甲酸酯类防腐剂[J].食品与发酵工业,2016,42(11):206-211.
[22]宗珊盈,李超,张娟,等.超高效液相色谱-串联质谱法同时测定食品中7种防腐剂和4种甜味剂[J].中国食品添加剂,2016(6):195-199.
[23]张璐,孔祥虹,李建华,等.固相萃取-超高效液相色谱-电喷雾串联质谱法同时测定食品中13种抗氧化剂[J].分析试验室,2014,33(1):43-47.
[24]HE Z,WANG L,PENG Y,et al.Multiresidue analysis of over 200 pesticides in cereals using a Qu ECh ERS and gas chromatography-tandem mass spectrometry-based method[J].Food Chemistry,2015,169:372-380.
[25]JIA W,LING Y,LIN Y,et al.Analysis of additives in dairy products by liquid chromatography coupled to quadrupole-orbitrap mass spectrometry[J].J Chromatogr A,2014,1 336(7):67-75.
[26]粟有志,马晓雯,孟茹,等.Qu ECh ERS-高效液相色谱-串联质谱法测定酵母抽提物中9种黄色合成色素[J].分析科学学报,2016,32(2):234-238.