超高效液相串联四级杆-飞行时间质谱快速测定食品原料中的氯化血红素
|
摘要
利用超高效液相串联四级杆-飞行时间质谱联用仪建立了氯化血红素的定性、定量分析方法。采用电喷雾离子源在质谱多反应监测正离子模式下对氯化血红素进行研究。实验测得氯化血红素信号最强的特征离子对为616→557,且质量浓度在2. 5～100 mg/L具有良好的线性关系。该定量方法的检测限和定量限分别为1. 25μg/L和4. 00μg/L,回收率80. 65%～102. 99%,精密度为3. 84%。该方法能有效用于保健品中氯化血红素的定性、定量分析。
A rapid and sensitive qualitative and quantitative analysis method for hemin by ultra-high performance liquid chromatography-quadrupole time-of-flight tandem mass spectrometry( UHPLC-QTOF-MS) was established. The electrospray ion source was used for studying hemin at mass spectrometry multiple reaction monitoring positive ion mode. The characteristic ion pair with the strongest hemin signal was 616→557,and there was a good linear relationship in the range of 2. 5-100 mg/L. The detection and quantitation limits of the method were 1. 25 μg/L and 4. 0μg/L,respectively. The recovery rate ranged from 80. 65% to 102. 99%,and the precision was 3. 84%. The results show that the method has high recovery rate and good precision,and therefore can be effectively used for quantitative and qualitative analysis of hemin in health care products.
A rapid and sensitive qualitative and quantitative analysis method for hemin by ultra-high performance liquid chromatography-quadrupole time-of-flight tandem mass spectrometry( UHPLC-QTOF-MS) was established. The electrospray ion source was used for studying hemin at mass spectrometry multiple reaction monitoring positive ion mode. The characteristic ion pair with the strongest hemin signal was 616→557,and there was a good linear relationship in the range of 2. 5-100 mg/L. The detection and quantitation limits of the method were 1. 25 μg/L and 4. 0μg/L,respectively. The recovery rate ranged from 80. 65% to 102. 99%,and the precision was 3. 84%. The results show that the method has high recovery rate and good precision,and therefore can be effectively used for quantitative and qualitative analysis of hemin in health care products.
引文
[1]张慧群.血红素的催化性质以及抗氧化性能的研究[D].西安:西北大学,2015.
[2]王传清,袁弥满.氯化高铁血红素对正常及再生障碍性贫血小鼠红系祖细胞的体内诱导作用[J].中华血液学杂志,1998,19(10):507-509.
[3]宋照军,刘蜜,赵良,等.血红素提取纯化新技术研究[J].广州食品工业科技,2003,20(8):6-8.
[4]朱天强,杨华,王冰,等.氯代血红素的多级质谱研究(MS1~MS7)[J].分析测试学报,2004,23(5):78-81.
[5]刘凡,张元勤.氯化血红素与牛血清白蛋白的作用及表面活性剂对其的影响研究[J].四川师范大学学报(自然科学版),2012,35(3):386-390.
[6]霍仕霞,闫明,黄毅,等. HPLC法测定氯化血红素片剂的含量[J].分析试验室,2008,27(S1):227-229.
[7]李得加,安玉会,张旭,等.有机介质中氯化血红素催化邻苯二胺氧化反应的研究[J].郑州大学学报(理学版),2007,39(1):101-106.
[8]黄应平,方艳芬,许文年,等.模拟酶催化反应用于环境样品中苯酚的测定[J].分析科学学报,2008,24(1):51-54.
[9] TOUSSON E,ALI E M,IBRAHIM W,et al. Histopathological and immunohistochemical alterations in rat heart after thyroidectomy and the role of hemin and ketoconazole in treatment[J]. Biomedicine&Pharmacotherapy,2012,66(8):627-632.
[10]李兴春.氯化血红素的性质和检测方法[J].中国生化药物杂志,1993(4):58-59.
[11] MESSORI L,PICCIOLI F,EITLERB,et al. Spectrophotometric and ESI-MS/HPLC studies reveal a common mechanism for the reaction of various artemisinin analogues with hemin[J]. Bioorganic&Medicinal Chemistry Letters,2003,13(22):4 055-4 057.
[12]何云华,聂峰.流动注射化学发光法测定氯化血红素[J].分析试验室,2008,27(7):39-42.
[13] LIU K,SONG Y,LIU Y. et al. An integrated strategy using UPLC-QTOF-MSEand UPLC-QTOF-MRM(enhanced target)for pharmacokinetics study of wine processed schisandra chinensis fructus in rats[J]. Journal of Pharmaceutical&Biomedical Analysis,2017,139:165-178.
[14]洪健,周大寨,唐巧玉.超高压液相色谱-飞行时间质谱联用快速测定酒中3种甜味剂[J].湖北民族学院学报(自然科学版),2017,35(2):162-166.
[15] CAJKA T,HAJSLOVA'J. Gas chromatography-high-resolution time-of-flight mass spectrometry in pesticide residue analysis:Advantages and limitations[J]. Journal of Chromatography A,2004,1058(1):251-261.
[16]杨术鹏,王莹,李彦伸,等.超高效液相色谱串联四级杆/飞行时间质谱仪鉴定喹赛多在鸡体内代谢研究[J].中国畜牧兽医,2013,40(3):11-19.
[17]王卉,陆安祥,韩平,等.超高效液相色谱-串联四级杆/飞行时间质谱法在饮用水检测中的应用[J].食品安全质量检测学报,2016(11):4 467-4 471.
[18] TAO W,LV H,WANG F,et al. Characterization of polyphenols from Lycium ruthenicum fruit by UPLC-QTOF/MSE and their antioxidant activity in caco-2 cells[J]. Journal of Agricultural&Food Chemistry,2016,64(11):2 280.
[19] XU B,ZHANG D Y,LIU Z Y,et al. Rapid determination of 1-deoxynojirimycin in Morus alba L. leaves by direct analysis in real time(DART)mass spectrometry[J]. Journal of Pharmaceutical&Biomedical Analysis,2015,114:447-454.
[20] DU P,WU X,XU J,et al. Determination and dissipation of mesotrione and its metabolites in rice using UPLC and triple-quadrupole tandem mass spectrometry[J]. Food Chemistry,2017,229:260-267.
[21] CHENG Y,DONG F,LIU X,et al. Simultaneous determination of fipronil and its major metabolites in corn and soil by ultra-performance liquid chromatography-tandem mass spectrometry[J]. Analytical Methods,2014,6(6):1 788-1 795.
[22] LU Z,FANG N,ZHANG Z,et al. Simultaneous determination of five neonicotinoid insecticides in edible fungi using ultrahigh-performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)[J]. Food Analytical Methods,2018,11(4):1 086-1 094.
[23]胡曙光,龙朝阳,梁旭霞,等.高效液相色谱法测定食品中氯化血红素含量[J].华南预防医学,2012(1):73-74.
[24] SANTE/11945/2015-Guidance document on analytical quality control and method validation procedures for pesticides residues analysis in food and feed[S]. European Commission,2016.
[25] KACZYN'SKI P. Clean-up and matrix effect in LC-MS/MS analysis of food of plant origin for high polar herbicides[J]. Food Chemistry,2017,230:524.
[2]王传清,袁弥满.氯化高铁血红素对正常及再生障碍性贫血小鼠红系祖细胞的体内诱导作用[J].中华血液学杂志,1998,19(10):507-509.
[3]宋照军,刘蜜,赵良,等.血红素提取纯化新技术研究[J].广州食品工业科技,2003,20(8):6-8.
[4]朱天强,杨华,王冰,等.氯代血红素的多级质谱研究(MS1~MS7)[J].分析测试学报,2004,23(5):78-81.
[5]刘凡,张元勤.氯化血红素与牛血清白蛋白的作用及表面活性剂对其的影响研究[J].四川师范大学学报(自然科学版),2012,35(3):386-390.
[6]霍仕霞,闫明,黄毅,等. HPLC法测定氯化血红素片剂的含量[J].分析试验室,2008,27(S1):227-229.
[7]李得加,安玉会,张旭,等.有机介质中氯化血红素催化邻苯二胺氧化反应的研究[J].郑州大学学报(理学版),2007,39(1):101-106.
[8]黄应平,方艳芬,许文年,等.模拟酶催化反应用于环境样品中苯酚的测定[J].分析科学学报,2008,24(1):51-54.
[9] TOUSSON E,ALI E M,IBRAHIM W,et al. Histopathological and immunohistochemical alterations in rat heart after thyroidectomy and the role of hemin and ketoconazole in treatment[J]. Biomedicine&Pharmacotherapy,2012,66(8):627-632.
[10]李兴春.氯化血红素的性质和检测方法[J].中国生化药物杂志,1993(4):58-59.
[11] MESSORI L,PICCIOLI F,EITLERB,et al. Spectrophotometric and ESI-MS/HPLC studies reveal a common mechanism for the reaction of various artemisinin analogues with hemin[J]. Bioorganic&Medicinal Chemistry Letters,2003,13(22):4 055-4 057.
[12]何云华,聂峰.流动注射化学发光法测定氯化血红素[J].分析试验室,2008,27(7):39-42.
[13] LIU K,SONG Y,LIU Y. et al. An integrated strategy using UPLC-QTOF-MSEand UPLC-QTOF-MRM(enhanced target)for pharmacokinetics study of wine processed schisandra chinensis fructus in rats[J]. Journal of Pharmaceutical&Biomedical Analysis,2017,139:165-178.
[14]洪健,周大寨,唐巧玉.超高压液相色谱-飞行时间质谱联用快速测定酒中3种甜味剂[J].湖北民族学院学报(自然科学版),2017,35(2):162-166.
[15] CAJKA T,HAJSLOVA'J. Gas chromatography-high-resolution time-of-flight mass spectrometry in pesticide residue analysis:Advantages and limitations[J]. Journal of Chromatography A,2004,1058(1):251-261.
[16]杨术鹏,王莹,李彦伸,等.超高效液相色谱串联四级杆/飞行时间质谱仪鉴定喹赛多在鸡体内代谢研究[J].中国畜牧兽医,2013,40(3):11-19.
[17]王卉,陆安祥,韩平,等.超高效液相色谱-串联四级杆/飞行时间质谱法在饮用水检测中的应用[J].食品安全质量检测学报,2016(11):4 467-4 471.
[18] TAO W,LV H,WANG F,et al. Characterization of polyphenols from Lycium ruthenicum fruit by UPLC-QTOF/MSE and their antioxidant activity in caco-2 cells[J]. Journal of Agricultural&Food Chemistry,2016,64(11):2 280.
[19] XU B,ZHANG D Y,LIU Z Y,et al. Rapid determination of 1-deoxynojirimycin in Morus alba L. leaves by direct analysis in real time(DART)mass spectrometry[J]. Journal of Pharmaceutical&Biomedical Analysis,2015,114:447-454.
[20] DU P,WU X,XU J,et al. Determination and dissipation of mesotrione and its metabolites in rice using UPLC and triple-quadrupole tandem mass spectrometry[J]. Food Chemistry,2017,229:260-267.
[21] CHENG Y,DONG F,LIU X,et al. Simultaneous determination of fipronil and its major metabolites in corn and soil by ultra-performance liquid chromatography-tandem mass spectrometry[J]. Analytical Methods,2014,6(6):1 788-1 795.
[22] LU Z,FANG N,ZHANG Z,et al. Simultaneous determination of five neonicotinoid insecticides in edible fungi using ultrahigh-performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)[J]. Food Analytical Methods,2018,11(4):1 086-1 094.
[23]胡曙光,龙朝阳,梁旭霞,等.高效液相色谱法测定食品中氯化血红素含量[J].华南预防医学,2012(1):73-74.
[24] SANTE/11945/2015-Guidance document on analytical quality control and method validation procedures for pesticides residues analysis in food and feed[S]. European Commission,2016.
[25] KACZYN'SKI P. Clean-up and matrix effect in LC-MS/MS analysis of food of plant origin for high polar herbicides[J]. Food Chemistry,2017,230:524.