亲水性液相色谱串联质谱法测定红甜菜中甜菜碱含量
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摘要
为了建立红甜菜中甜菜碱的定量分析方法,采用改进的QuEChERS方法结合液相色谱串联质谱技术,样品经快速溶剂萃取仪以甲醇为溶剂提取,经固相萃取柱净化,采用正向亲水性液相色谱柱(Hilic),梯度洗脱,通过质谱的多反应监测(multiple reactions monitoring, MRM)正离子模式扫描进行测定,外标法定量。结果表明:甜菜碱在本方法的线性范围为0.05～5μg/mL,添加水平为4～16 mg/g时,回收率为87.7%～95.7%,方法RSD值为3.69%～8.4%,检出限为0.01 mg/L,定量限为0.04 mg/L,与传统的分析方法相比,具有检出限低、灵敏度高的优点,完全可以适用于甜菜中甜菜碱的分析。
The study aims to establish a quantitative analysis method for detecting betaine in red sugarbeet.By using the modified QuEChERS method combined with liquid chromatography-tandem mass spectrometry,the sample was extracted with methanol through accelerated solvent extraction(ASE),and purified by solid phase extraction,detected by hydrophilic interaction liquid chromatography-tandem mass spectrometry under multiple reaction monitoring mode and quantified by the external standard method.The results showed that linearity range was 0.05-5 μg/mL in the test.When the adding level was 4-16 mg/g,the recovery was 87.7%-95.7%,and RSD was between 3.6% and 8.4%.The limit of detection(LOD) and the limit of quantification(LOQ) were 0.01 and 0.04 mg/L,respectively.The method is easy,quick,highly sensitive,and suitable for determination of betaine in sugabeet.
The study aims to establish a quantitative analysis method for detecting betaine in red sugarbeet.By using the modified QuEChERS method combined with liquid chromatography-tandem mass spectrometry,the sample was extracted with methanol through accelerated solvent extraction(ASE),and purified by solid phase extraction,detected by hydrophilic interaction liquid chromatography-tandem mass spectrometry under multiple reaction monitoring mode and quantified by the external standard method.The results showed that linearity range was 0.05-5 μg/mL in the test.When the adding level was 4-16 mg/g,the recovery was 87.7%-95.7%,and RSD was between 3.6% and 8.4%.The limit of detection(LOD) and the limit of quantification(LOQ) were 0.01 and 0.04 mg/L,respectively.The method is easy,quick,highly sensitive,and suitable for determination of betaine in sugabeet.
引文
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[2] Li T, Cui Y, Mathaga J, et al. Hydration and vibrational dynamics ofbetaine(N,N,N-trimethylglycine)[J].Journal of Chemical Physics,2015,142(21):1346.
[3] Liu J, Zhao M, Zhou J, et al. Simultaneous targeted analysis oftrimethylamine-N-oxide, choline, betaine, and carnitine by highperformance liquid chromatography tandem mass spectrometry[J].JChromatogr B Analyt Technol Biomed Life Sci,2016,1035:42-48.
[4]梁景辉,贾芙蓉,时璐,等.HPLC-ELSD测定枸杞子中甜菜碱的含量[J].中国处方药,2016(2):32-33.
[5] Mi S, Zhao Y Y, Jacobs R L, et al. Simultaneous determination oftrimethylamine and trimethylamine N-oxide in mouse plasmasamples by hydrophilic interaction liquid chromatography coupledto tandem mass spectrometry[J].Journal of Separation Science,2017,40(3):688.
[6] Mostafalu R, Banaei A, Ghorbani F. An Inaccuracy in theDetermination of Cocoamidopropyl Betaine by the PotentiometricMethod[J].Journal of Surfactants&Detergents,2015,18(5):919-922.
[7] Merkova M, Zalesak M, Ringlova E, et al. Degradation of thesurfactant Cocamidopropyl betaine by two bacterial strains isolatedfrom activated sludge[J].International Biodeterioration&Biodegradation,2018,127:236-240.
[8] Gholami A, Golestaneh M, Andalib Z. A new method fordetermination of cocamidopropyl betaine synthesized from coconutoil through spectral shift of Eriochrome Black T.[J].SpectrochimicaActa Part A Molecular&Biomolecular Spectroscopy,2017,192:122-127.
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[10]刘英华,杨晓华,王玉春.小麦叶片中甘氨酸甜菜碱含量的毛细管电泳测定方法研究[J].麦类作物学报,2007,27(4):717-720.
[11]王思威,刘艳萍,孙海滨.超高效液相色谱-串联质谱法测定荔枝花粉花蜜中吡唑醚菌酯及其代谢物[J].分析化学,2018(5):704-709.
[12]谢景梦,孟辰颖,李二粉,等.液相色谱串联质谱同时监测猪尿中10种违禁药物[J].分析化学,2018(5):750-756.
[13] Slow S, Donaggio M, Cressey P J, et al. The betaine content of NewZealand foods and estimated intake in the New Zealand diet[J].Journal of Food Composition&Analysis,2005,18(6):473-485.
[14]宋晓娟,李海燕,尹明明,等.快速溶剂萃取-气相色谱-串联质谱法分析海洋沉积物中16种多环芳烃[J].色谱,2018,36(1):51-58.
[15]闫蕊,邵明媛,鞠福龙,等.加速溶剂萃取-高效液相色谱串联质谱法测定土壤中农药残留[J].分析化学,2013,41(2):315-316.
[16]王少娟,董军,周鹏娜.快速溶剂萃取与索氏抽提对比测定复垦土壤中4类20种半挥发性有机污染物[J].分析试验室,2018,37(04):404-408.
[17]纪律,徐峻卿,李启,等.快速溶剂萃取-超高效液相色谱串联质谱法测定竹笋中的百草枯残留[J].中国卫生检验杂志,2018,28(1):18-21.
[18]金党琴,丁邦东,龚爱琴,等.快速溶剂萃取高效液相色谱法测定蔬菜中烯禾啶和麦草畏残留[J].化学试剂,2018,40(4):357-360.
[19]唐巧玉,周毅峰.快速溶剂萃取法提取水芹中总黄酮工艺研究[J].食品科学,2010,31(22):190-193.
[20]宋国胜,胡松青,李琳.超声波技术在食品科学中的应用与研究[J].现代食品科技,2008,24(6):609-612.
[21]胡建平,罗舒月.葛根中黄酮提取工艺的研究[J].食品工业科技,2008,29(8):227-234.
[22] Day C R. Betaine chemistry, roles, and potential use in liver disease[J].Biochim Biophys Acta,2016,1860(6):1098-1106.
[23] Holm P I, Ueland P M, Kvalheim G, et al. Determination ofcholine,betaine, and dimethylglycine in plasma by a high-throughputmethod based on normal-phase chromatography-tan-dem massspectrometry[J].Clin Chem.,2003,49(2):286-294.
[24] Rivoira L, Studzińska S, Szultka-M?yńska M, et al. Newapproaches for extraction and determination of betaine from Betavulgaris samples by hydrophilic interaction liquid chromatography-tandem mass spectrometry[J].Analytical&Bioanalytical Chemistry,2017,409(21):5133-5141.
[25]刘正才,张琼,杨方,等.亲水作用色谱-电喷雾串联质谱法测定水产品中的氟苯尼考胺的残留量[J].食品科学,2015,36(4):198-201.
[26] Shrivastava A, Gupta V B. Methods for the determination of limitof detection and limit of quantitation of the analytical methods[J].Chronicles of Young Scientists,2011,2(1):21-25.
[27]张弦飞.超高效合相色谱-串联质谱法快速测定枸杞中甜菜碱含量(英文)[J].色谱,2018,36(5):417-424.
[2] Li T, Cui Y, Mathaga J, et al. Hydration and vibrational dynamics ofbetaine(N,N,N-trimethylglycine)[J].Journal of Chemical Physics,2015,142(21):1346.
[3] Liu J, Zhao M, Zhou J, et al. Simultaneous targeted analysis oftrimethylamine-N-oxide, choline, betaine, and carnitine by highperformance liquid chromatography tandem mass spectrometry[J].JChromatogr B Analyt Technol Biomed Life Sci,2016,1035:42-48.
[4]梁景辉,贾芙蓉,时璐,等.HPLC-ELSD测定枸杞子中甜菜碱的含量[J].中国处方药,2016(2):32-33.
[5] Mi S, Zhao Y Y, Jacobs R L, et al. Simultaneous determination oftrimethylamine and trimethylamine N-oxide in mouse plasmasamples by hydrophilic interaction liquid chromatography coupledto tandem mass spectrometry[J].Journal of Separation Science,2017,40(3):688.
[6] Mostafalu R, Banaei A, Ghorbani F. An Inaccuracy in theDetermination of Cocoamidopropyl Betaine by the PotentiometricMethod[J].Journal of Surfactants&Detergents,2015,18(5):919-922.
[7] Merkova M, Zalesak M, Ringlova E, et al. Degradation of thesurfactant Cocamidopropyl betaine by two bacterial strains isolatedfrom activated sludge[J].International Biodeterioration&Biodegradation,2018,127:236-240.
[8] Gholami A, Golestaneh M, Andalib Z. A new method fordetermination of cocamidopropyl betaine synthesized from coconutoil through spectral shift of Eriochrome Black T.[J].SpectrochimicaActa Part A Molecular&Biomolecular Spectroscopy,2017,192:122-127.
[9]龚立冬,曹玉华,侯建霞.高效液相色谱-蒸发光散射检测法测定肉苁蓉中的甜菜碱[J].色谱,2007,25(2):280-281.
[10]刘英华,杨晓华,王玉春.小麦叶片中甘氨酸甜菜碱含量的毛细管电泳测定方法研究[J].麦类作物学报,2007,27(4):717-720.
[11]王思威,刘艳萍,孙海滨.超高效液相色谱-串联质谱法测定荔枝花粉花蜜中吡唑醚菌酯及其代谢物[J].分析化学,2018(5):704-709.
[12]谢景梦,孟辰颖,李二粉,等.液相色谱串联质谱同时监测猪尿中10种违禁药物[J].分析化学,2018(5):750-756.
[13] Slow S, Donaggio M, Cressey P J, et al. The betaine content of NewZealand foods and estimated intake in the New Zealand diet[J].Journal of Food Composition&Analysis,2005,18(6):473-485.
[14]宋晓娟,李海燕,尹明明,等.快速溶剂萃取-气相色谱-串联质谱法分析海洋沉积物中16种多环芳烃[J].色谱,2018,36(1):51-58.
[15]闫蕊,邵明媛,鞠福龙,等.加速溶剂萃取-高效液相色谱串联质谱法测定土壤中农药残留[J].分析化学,2013,41(2):315-316.
[16]王少娟,董军,周鹏娜.快速溶剂萃取与索氏抽提对比测定复垦土壤中4类20种半挥发性有机污染物[J].分析试验室,2018,37(04):404-408.
[17]纪律,徐峻卿,李启,等.快速溶剂萃取-超高效液相色谱串联质谱法测定竹笋中的百草枯残留[J].中国卫生检验杂志,2018,28(1):18-21.
[18]金党琴,丁邦东,龚爱琴,等.快速溶剂萃取高效液相色谱法测定蔬菜中烯禾啶和麦草畏残留[J].化学试剂,2018,40(4):357-360.
[19]唐巧玉,周毅峰.快速溶剂萃取法提取水芹中总黄酮工艺研究[J].食品科学,2010,31(22):190-193.
[20]宋国胜,胡松青,李琳.超声波技术在食品科学中的应用与研究[J].现代食品科技,2008,24(6):609-612.
[21]胡建平,罗舒月.葛根中黄酮提取工艺的研究[J].食品工业科技,2008,29(8):227-234.
[22] Day C R. Betaine chemistry, roles, and potential use in liver disease[J].Biochim Biophys Acta,2016,1860(6):1098-1106.
[23] Holm P I, Ueland P M, Kvalheim G, et al. Determination ofcholine,betaine, and dimethylglycine in plasma by a high-throughputmethod based on normal-phase chromatography-tan-dem massspectrometry[J].Clin Chem.,2003,49(2):286-294.
[24] Rivoira L, Studzińska S, Szultka-M?yńska M, et al. Newapproaches for extraction and determination of betaine from Betavulgaris samples by hydrophilic interaction liquid chromatography-tandem mass spectrometry[J].Analytical&Bioanalytical Chemistry,2017,409(21):5133-5141.
[25]刘正才,张琼,杨方,等.亲水作用色谱-电喷雾串联质谱法测定水产品中的氟苯尼考胺的残留量[J].食品科学,2015,36(4):198-201.
[26] Shrivastava A, Gupta V B. Methods for the determination of limitof detection and limit of quantitation of the analytical methods[J].Chronicles of Young Scientists,2011,2(1):21-25.
[27]张弦飞.超高效合相色谱-串联质谱法快速测定枸杞中甜菜碱含量(英文)[J].色谱,2018,36(5):417-424.