超高效液相串联质谱检测茶叶及茶饮料中咖啡因含量
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摘要
建立超高效液相串联质谱检测茶叶及茶饮料中咖啡因含量的方法。茶叶及茶饮料经前处理后进样,以0.1%甲酸水溶液-乙腈(80∶20,v/v)为流动相等度洗脱,流速为0.3 m L/min,经C_(18)色谱柱分离,柱温25℃;质谱采用电喷雾离子源正离子模式、多反应检测模式检测,脱溶剂气(N_2)温度500℃、流速700 L/Hr,毛细管电压3.5 k V,锥孔电压55 V,碰撞气为高纯氩气。在上述分析条件下,本法咖啡因的检出限为2.0μg/L;在2.0～1000μg/L浓度范围内的线性关系良好,相关系数r为0.9969;加标回收率达90.2%～103.9%;相对标准偏差在1.00%～3.00%(n=6)。本方法简便、快速,选择性、重现性好、灵敏度高,适用于茶叶及茶饮料中咖啡因的定量分析,结果准确可靠,对于复杂样品中咖啡因的检测有明显优势。
A new method,ultra-lipid chromatography-tandem mass spectrometry,which was used to exam the caffeine in tea and tea drinks,was developed in this experiment. After tea and tea drinks being pretreated,samples were separated by C_(18) column and the column temperature was 25 ℃ with 0.1% formic acid solution-acetonitrile( 80∶ 20,v/v) as the mobile phase for gradient elution,and the flow rate was set at 0.3 m L/min.The electrospray ionization source of MS in positive ion mode was used for multiple reaction monitoring,under conditions included that desolvation gas( N_2) temperature was 500 ℃ and the flow rate was 700 L/Hr,capillary voltage was 3.5 kV,cone voltage was 55 V and collision gas was high purity argon. Under conditions above,the limit of detection( LOD) of caffeine was 2.0 μg/L. There was a perfect linear relationship in relative concentration range( 2.0～1000 μg/L),and the correlation( r) was 0.9969,average recoveries were in the range from 90.2% to103.9%,and relative standard deviations( RSDs) were among 1.00% to 3.00%( n = 6).The established method was convenient,fast and had good selectivity,good reproducibility and high sensitivity. It was suitable for quantifying caffeine in tea and tea drinks,the method was accurate and reliable,and had an advantage in detecting caffeine contained in complex samples.
A new method,ultra-lipid chromatography-tandem mass spectrometry,which was used to exam the caffeine in tea and tea drinks,was developed in this experiment. After tea and tea drinks being pretreated,samples were separated by C_(18) column and the column temperature was 25 ℃ with 0.1% formic acid solution-acetonitrile( 80∶ 20,v/v) as the mobile phase for gradient elution,and the flow rate was set at 0.3 m L/min.The electrospray ionization source of MS in positive ion mode was used for multiple reaction monitoring,under conditions included that desolvation gas( N_2) temperature was 500 ℃ and the flow rate was 700 L/Hr,capillary voltage was 3.5 kV,cone voltage was 55 V and collision gas was high purity argon. Under conditions above,the limit of detection( LOD) of caffeine was 2.0 μg/L. There was a perfect linear relationship in relative concentration range( 2.0～1000 μg/L),and the correlation( r) was 0.9969,average recoveries were in the range from 90.2% to103.9%,and relative standard deviations( RSDs) were among 1.00% to 3.00%( n = 6).The established method was convenient,fast and had good selectivity,good reproducibility and high sensitivity. It was suitable for quantifying caffeine in tea and tea drinks,the method was accurate and reliable,and had an advantage in detecting caffeine contained in complex samples.
引文
[1]Joseph G L,Grace E L,Clifford H W.Caffeine concentrations in coffee,tea,chocolate,and energy drink flavored E-liquids[J].Nicotine Tobacco Research,2017,4(19):484-492.
[2]陈彩云,魏鲜娥,蔡伟江,等.液相色谱-串联质谱法测定巴西绿蜂胶制品中咖啡因含量[J].食品安全质量检测学报,2018,9(9):2212-2216.
[3]Yamanchi Y,Nakamura A,Kohno L,et al.Simple and rapid UV spectrophotometry of caffeine in tea coupled with sample retreatment using a cartridge column filled with polyvinylpolypyrolidone(PVPP)[J]. Chemical Pharmaceutical Bulletin,2008,56(2):185-188.
[4]Costa M S,Botton P H,Mioranzza S,et al.Caffeine prevents age-associated recognition memory decline and changes brainderived neurotrophic factor and tyrosine kinase receptor(Trk B)content in mice[J].Neuroscience,2008,153(4):1071-1078.
[5]Concerto C,Conti C,Battaqlia F. Sleep quality,perceived stress and caffeinated drinks intake in psychiatry residents:A cross-sectional study[J].Journal Caffeine Research,2017,7(1):18-22.
[6]Watson E J,Banks S,Coates A M,et al. The relationship between caffeine,sleep and behavior in children[J].Journal of Clinical Sleep Medicine,2017,13(4):533-543.
[7]Castellanos F X,Rapoport J L. Effects of caffeine on development and behavior in infancy and childhood:A review of the published literature[J].Food and Chemical Toxicology,2002,9(40):1235-1242.
[8]Shilo L,Sabbah H,Hadari R,et al. The effects of coffee consumption on sleep and melatonin sectretion[J]. Sleep Medicine,2002,3:271-273.
[9]Wen W Q,Shu X O,Jacobs D R,et al. The associations of maternal caffeine consumption and nausea with spontaneous abortion[J].Epidemology,2001(1):38-42.
[10]刘紫燕,刘政权,李真.超临界CO2脱除绿茶咖啡碱过程中茶叶香气变化研究[J].食品工业科技,2015(19):286-289.
[11]张明月,夏义平.茶饮料中咖啡因检测存在问题的探讨与研究[J].中国卫生检验杂志,2014,24(11):1560-1562.
[12]Showkat A B,Sim S F,Mohamad N M I.Spectrophotometric analysis of caffeine[J]. International Journal of Analytical Chemistry,2016,2015(6):170239.
[13]李蔚,李凤华,赵秀香.高效液相色谱法测定饮品中咖啡因[J].中国卫生检验杂志,2014,24(19):2787-2790.
[14]孙延春,张英.紫外光谱法测定饮料中的咖啡因含量[J].化学研究,2011,22(1):77-79.
[15]Verenitch S S,Mazumder A.Development of a methodology utilizing gas chromatography ion-trap tandem mass spectrometry for the determination of low levels of caffeine in surface marine and freshwater samples[J].Analytical and Bioanalytical Chemistry,2008,39(7):2635-2646.
[16]Turak F,Guzel R,Dinc E,et al.Simultaneous determination of ascorbic acid and caffeine in commercial soft drinks using revered-phase ultraperformance liquid chromatography[J].Journal of Food and Drug Analysis,2017,25(2):285-292.
[17]杨清山,蔡荣华,徐猛,等.UPLC法测定咖啡豆中绿原酸和咖啡因的含量[J].食品研究与开发,2015,36(18):138-140.
[18]徐丹萍,艾凌艳,夏小凤.高效液相色谱法测定潽耳熟沱茶叶中咖啡因的含量[J].海峡药学,2016,28(8):63-66.
[19]凌云,赵云峰,李志军,等.茶叶及茶饮料中儿茶素和咖啡因的多组分HPLC分析方法[J].卫生研究,2005,34(2):187-190.
[20]董树国,陆钊.高效液相色谱法测定绿茶饮料中的咖啡因含量[J].广东化工,2011,38(12):136-137.
[21]王嘉琦,贾丽,夏敏.液相色谱法测定饮料中咖啡因、可可碱和茶碱[J].现代食品科技,2011,27(1):114-116.
[22]邵华,刘有平,王鑫,等.液相色谱-大气压化学电离-串联质谱法同时测定人血浆中氯苯那敏和咖啡因的含量[J].沈阳药科大学学报,2009,26(5):388-392.
[23]GB 5009.139-2014饮料中咖啡因的测定[S].北京:中国标准出版社,2015:8.
[24]李婷,吕春秀,陈峰,等.脱咖啡因绿茶汤与普通绿茶汤的品质对比分析[J].食品研究与开发,2018,39(4):157-162.
[25]陈连清,陈玉,周忠强,等.核磁共振法无损伤测定茶叶中咖啡因含量研究型实验教学初探[J].实验室科学,2015,18(2):31-34.
[26]张文珠,王添爽,赵洋,等.测定饮料中咖啡因含量的综合性实验[J].实验室研究与探索,2016,35(1):13-15.
[27]曾诚,赵文惠.反相高效液相色谱和超高效液相色谱法测定饮料中咖啡因含量的比较研究[J].食品安全质量检测学报,2015,6(6):2337-2341.
[28]董丽丽,王秀玲.某些功能性饮料中咖啡因的快速检测方法研究[J].化学研究与应用,2013,25(9):1308-1313.
[29]Sereshti H,Samadi S. A rapid and simple determination of caffeine in teas,coffees and eight beverages[J].Food Chemistry,2014,158:8-13.
[30]GB/T27404-2008实验室质量控制规范食品理化检测[S].北京:中国标准出版社,2008:32.
[2]陈彩云,魏鲜娥,蔡伟江,等.液相色谱-串联质谱法测定巴西绿蜂胶制品中咖啡因含量[J].食品安全质量检测学报,2018,9(9):2212-2216.
[3]Yamanchi Y,Nakamura A,Kohno L,et al.Simple and rapid UV spectrophotometry of caffeine in tea coupled with sample retreatment using a cartridge column filled with polyvinylpolypyrolidone(PVPP)[J]. Chemical Pharmaceutical Bulletin,2008,56(2):185-188.
[4]Costa M S,Botton P H,Mioranzza S,et al.Caffeine prevents age-associated recognition memory decline and changes brainderived neurotrophic factor and tyrosine kinase receptor(Trk B)content in mice[J].Neuroscience,2008,153(4):1071-1078.
[5]Concerto C,Conti C,Battaqlia F. Sleep quality,perceived stress and caffeinated drinks intake in psychiatry residents:A cross-sectional study[J].Journal Caffeine Research,2017,7(1):18-22.
[6]Watson E J,Banks S,Coates A M,et al. The relationship between caffeine,sleep and behavior in children[J].Journal of Clinical Sleep Medicine,2017,13(4):533-543.
[7]Castellanos F X,Rapoport J L. Effects of caffeine on development and behavior in infancy and childhood:A review of the published literature[J].Food and Chemical Toxicology,2002,9(40):1235-1242.
[8]Shilo L,Sabbah H,Hadari R,et al. The effects of coffee consumption on sleep and melatonin sectretion[J]. Sleep Medicine,2002,3:271-273.
[9]Wen W Q,Shu X O,Jacobs D R,et al. The associations of maternal caffeine consumption and nausea with spontaneous abortion[J].Epidemology,2001(1):38-42.
[10]刘紫燕,刘政权,李真.超临界CO2脱除绿茶咖啡碱过程中茶叶香气变化研究[J].食品工业科技,2015(19):286-289.
[11]张明月,夏义平.茶饮料中咖啡因检测存在问题的探讨与研究[J].中国卫生检验杂志,2014,24(11):1560-1562.
[12]Showkat A B,Sim S F,Mohamad N M I.Spectrophotometric analysis of caffeine[J]. International Journal of Analytical Chemistry,2016,2015(6):170239.
[13]李蔚,李凤华,赵秀香.高效液相色谱法测定饮品中咖啡因[J].中国卫生检验杂志,2014,24(19):2787-2790.
[14]孙延春,张英.紫外光谱法测定饮料中的咖啡因含量[J].化学研究,2011,22(1):77-79.
[15]Verenitch S S,Mazumder A.Development of a methodology utilizing gas chromatography ion-trap tandem mass spectrometry for the determination of low levels of caffeine in surface marine and freshwater samples[J].Analytical and Bioanalytical Chemistry,2008,39(7):2635-2646.
[16]Turak F,Guzel R,Dinc E,et al.Simultaneous determination of ascorbic acid and caffeine in commercial soft drinks using revered-phase ultraperformance liquid chromatography[J].Journal of Food and Drug Analysis,2017,25(2):285-292.
[17]杨清山,蔡荣华,徐猛,等.UPLC法测定咖啡豆中绿原酸和咖啡因的含量[J].食品研究与开发,2015,36(18):138-140.
[18]徐丹萍,艾凌艳,夏小凤.高效液相色谱法测定潽耳熟沱茶叶中咖啡因的含量[J].海峡药学,2016,28(8):63-66.
[19]凌云,赵云峰,李志军,等.茶叶及茶饮料中儿茶素和咖啡因的多组分HPLC分析方法[J].卫生研究,2005,34(2):187-190.
[20]董树国,陆钊.高效液相色谱法测定绿茶饮料中的咖啡因含量[J].广东化工,2011,38(12):136-137.
[21]王嘉琦,贾丽,夏敏.液相色谱法测定饮料中咖啡因、可可碱和茶碱[J].现代食品科技,2011,27(1):114-116.
[22]邵华,刘有平,王鑫,等.液相色谱-大气压化学电离-串联质谱法同时测定人血浆中氯苯那敏和咖啡因的含量[J].沈阳药科大学学报,2009,26(5):388-392.
[23]GB 5009.139-2014饮料中咖啡因的测定[S].北京:中国标准出版社,2015:8.
[24]李婷,吕春秀,陈峰,等.脱咖啡因绿茶汤与普通绿茶汤的品质对比分析[J].食品研究与开发,2018,39(4):157-162.
[25]陈连清,陈玉,周忠强,等.核磁共振法无损伤测定茶叶中咖啡因含量研究型实验教学初探[J].实验室科学,2015,18(2):31-34.
[26]张文珠,王添爽,赵洋,等.测定饮料中咖啡因含量的综合性实验[J].实验室研究与探索,2016,35(1):13-15.
[27]曾诚,赵文惠.反相高效液相色谱和超高效液相色谱法测定饮料中咖啡因含量的比较研究[J].食品安全质量检测学报,2015,6(6):2337-2341.
[28]董丽丽,王秀玲.某些功能性饮料中咖啡因的快速检测方法研究[J].化学研究与应用,2013,25(9):1308-1313.
[29]Sereshti H,Samadi S. A rapid and simple determination of caffeine in teas,coffees and eight beverages[J].Food Chemistry,2014,158:8-13.
[30]GB/T27404-2008实验室质量控制规范食品理化检测[S].北京:中国标准出版社,2008:32.