超高压液相色谱-四级杆-轨道阱质谱同时测定苦荞酒中的甜菜碱与葛根素
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摘要
目的建立苦荞酒中甜菜碱与葛根素的超高压液相色谱-四极杆-轨道阱质谱检测方法。方法苦荞酒经0. 22μm滤膜过滤、流动相(甲醇∶水=50∶50)稀释后,以C18柱(100 mm×2. 1 mm,1. 8μm)分离甜菜碱和葛根素。四极杆和轨道阱质谱检测,使用ESI源,一级与二级质谱同时检测。结果甜菜碱与葛根素达到良好分离,在100μg/L～2 000μg/L范围内线性良好,相关系数均大于0. 999。不同水平的加标回收率在96. 7%～98. 3%之间,相对标准偏差均小于2%。甜菜碱仪器检出限和定量限分别为0. 5μg/L和2. 0μg/L。葛根素仪器检出限和定量限分别为2. 0μg/L和5. 0μg/L。结论该方法快速、同时、准确,适用于苦荞酒中甜菜碱与葛根素的测定。
Objective To establish an analytical method for simultaneous determination of betaine and puerarin in buckwheat wine. Method Buckwheat wine was filtered by 0. 22 μm filter membrane and diluted by mobile phase( methanol: water = 50∶50),then betaine and puerarin were determined by ultra-high pressure liquid chromatography-quadrupole orbitrap mass spectrometry( ESI source) in full scan and MS2 mode. Results A good linear relationship( r > 0. 999) was observed with betaine and puerarin concentrations from 100 μg/L to 2 000 μg/L. The average recoveries at different levels of betaine and puerarin ranged from 96. 7 % to 98. 3 % with the relative standard deviations( RSD,n = 3) all smaller than 2%. The limits of detection( LOD,S/N = 3) and the limits of quantification( LOQ,S/N = 10) for betaine were 0. 5 μg/L and 2. 0 μg/L. The LOD and LOQ for puerarin were 2. 0 μg/L and 5. 0 μg/L. Conclusion This method is rapid,simultaneous and accurate. It is suitable for the determination of betaine and puerarin in the buckwheat wine.
Objective To establish an analytical method for simultaneous determination of betaine and puerarin in buckwheat wine. Method Buckwheat wine was filtered by 0. 22 μm filter membrane and diluted by mobile phase( methanol: water = 50∶50),then betaine and puerarin were determined by ultra-high pressure liquid chromatography-quadrupole orbitrap mass spectrometry( ESI source) in full scan and MS2 mode. Results A good linear relationship( r > 0. 999) was observed with betaine and puerarin concentrations from 100 μg/L to 2 000 μg/L. The average recoveries at different levels of betaine and puerarin ranged from 96. 7 % to 98. 3 % with the relative standard deviations( RSD,n = 3) all smaller than 2%. The limits of detection( LOD,S/N = 3) and the limits of quantification( LOQ,S/N = 10) for betaine were 0. 5 μg/L and 2. 0 μg/L. The LOD and LOQ for puerarin were 2. 0 μg/L and 5. 0 μg/L. Conclusion This method is rapid,simultaneous and accurate. It is suitable for the determination of betaine and puerarin in the buckwheat wine.
引文
[1]徐笑宇.高黄酮苦荞资源鉴选与评价利用研究[D].咸阳:西北农林科技大学,2015.
[2]Alfthan G,Tapani K,Nissinen K,et al.The effect of low doses of betaine on plasma homocysteine in healthy volunteers[J].The British Journal of Nutrition,2004,92(4):665-669.
[3]Khodayar MJ,Kalantari H,Khorsandi L,et al.Betaine protects mice against acetaminophen hepatotoxicity possibly via mitochondrial complex II and glutathione availability[J].Biomedicine&Pharmacotherapy,2018,103:1436-1445.
[4]Zhou RF,Chen XL,Zhou ZG,et al.Higher dietary intakes of choline and betaine are associated with a lower risk of primary liver cancer:a case-control study[J].Scientific Reports,2017,7(1):679.
[5]Deng HF,Wang S,Li L,et al.Puerarin prevents vascular endothelial injury through suppression of NF-κB activation in LPS-challenged human umbilical vein endothelial cells[J].Biomedicine&Pharmacotherapy,2018,104:261-267.
[6]Wan Q,Liu ZY,Yang YP.Puerarin inhibits vascular smooth muscle cells proliferation induced by fine particulate matter via suppressing of the p38 MAPK signaling pathway[J].BMC Complementary and Alternative Medicine,2018,18(1):146.
[7]Hu YF,Li X,Lin L,et al.Puerarin inhibits non-small cell lung cancer cell growth via the induction of apoptosis[J].Oncology Reports,2018,39(4):1731-1738.
[8]Pearce RB,Strange RN,Smith H.Glycinebetaine and choline in wheat:distribution and relation to infection by Fusarium graminearum[J].Phytochemistry,1976,15(6):953-954.
[9]朱桂花,杨高文,陈晓光.应用分光光度法测定枸杞半成品饮料中的甜菜碱含量[J].冷饮与速冻食品工业,1998(1):23-25.
[10]齐永秀,郝立勇,翟宏艳,等.非水滴定法测定盐酸甜菜碱的含量[J].泰山医学院学报,2002,23(4):355-356.
[11]郭辉,刘同祥,陈富君,等.薄层扫描法测定肝肾滋中甜菜碱的含量[J].中国中药杂志,2007,32(1):71-72.
[12]Rivoira L,Studzińska S,Szultka-M?yńska M,et al.New approaches for extraction and determination of betaine from Beta vulgaris samples by hydrophilic interaction liquid chromatographytandem mass spectrometry[J].Analytical and Bioanalytical Chemistry,2017,409(21):5133-5141.
[13]董孝元,喻斌,吴昊,等.苦荞酒中甜菜碱检测方法及抗氧化性研究[J].酿酒科技,2016,11(11):37-40.
[14]常颖,谭炳炎,郑琳,等.高效液相色谱法测定人血清甜菜碱方法的建立[J].中华检验医学杂志,2010,33(5):405-408.
[15]黄蘅,陈学松,廖强.HPLC-ELSD法测定枸杞子中甜菜碱[J].中国实验方剂学杂志,2010,16(7):59-60.
[16]Wang PG,Zhou W.Rapid determination of cocamidopropyl betaine impurities in cosmetic products by core-shell hydrophilic interaction liquid chromatography-tandem mass spectrometry[J].Journal of Chromatography A.,2016,1461:78-83.
[2]Alfthan G,Tapani K,Nissinen K,et al.The effect of low doses of betaine on plasma homocysteine in healthy volunteers[J].The British Journal of Nutrition,2004,92(4):665-669.
[3]Khodayar MJ,Kalantari H,Khorsandi L,et al.Betaine protects mice against acetaminophen hepatotoxicity possibly via mitochondrial complex II and glutathione availability[J].Biomedicine&Pharmacotherapy,2018,103:1436-1445.
[4]Zhou RF,Chen XL,Zhou ZG,et al.Higher dietary intakes of choline and betaine are associated with a lower risk of primary liver cancer:a case-control study[J].Scientific Reports,2017,7(1):679.
[5]Deng HF,Wang S,Li L,et al.Puerarin prevents vascular endothelial injury through suppression of NF-κB activation in LPS-challenged human umbilical vein endothelial cells[J].Biomedicine&Pharmacotherapy,2018,104:261-267.
[6]Wan Q,Liu ZY,Yang YP.Puerarin inhibits vascular smooth muscle cells proliferation induced by fine particulate matter via suppressing of the p38 MAPK signaling pathway[J].BMC Complementary and Alternative Medicine,2018,18(1):146.
[7]Hu YF,Li X,Lin L,et al.Puerarin inhibits non-small cell lung cancer cell growth via the induction of apoptosis[J].Oncology Reports,2018,39(4):1731-1738.
[8]Pearce RB,Strange RN,Smith H.Glycinebetaine and choline in wheat:distribution and relation to infection by Fusarium graminearum[J].Phytochemistry,1976,15(6):953-954.
[9]朱桂花,杨高文,陈晓光.应用分光光度法测定枸杞半成品饮料中的甜菜碱含量[J].冷饮与速冻食品工业,1998(1):23-25.
[10]齐永秀,郝立勇,翟宏艳,等.非水滴定法测定盐酸甜菜碱的含量[J].泰山医学院学报,2002,23(4):355-356.
[11]郭辉,刘同祥,陈富君,等.薄层扫描法测定肝肾滋中甜菜碱的含量[J].中国中药杂志,2007,32(1):71-72.
[12]Rivoira L,Studzińska S,Szultka-M?yńska M,et al.New approaches for extraction and determination of betaine from Beta vulgaris samples by hydrophilic interaction liquid chromatographytandem mass spectrometry[J].Analytical and Bioanalytical Chemistry,2017,409(21):5133-5141.
[13]董孝元,喻斌,吴昊,等.苦荞酒中甜菜碱检测方法及抗氧化性研究[J].酿酒科技,2016,11(11):37-40.
[14]常颖,谭炳炎,郑琳,等.高效液相色谱法测定人血清甜菜碱方法的建立[J].中华检验医学杂志,2010,33(5):405-408.
[15]黄蘅,陈学松,廖强.HPLC-ELSD法测定枸杞子中甜菜碱[J].中国实验方剂学杂志,2010,16(7):59-60.
[16]Wang PG,Zhou W.Rapid determination of cocamidopropyl betaine impurities in cosmetic products by core-shell hydrophilic interaction liquid chromatography-tandem mass spectrometry[J].Journal of Chromatography A.,2016,1461:78-83.