UPLC/MS/MS法定性定量测定中药材中3类27种合成色素
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摘要
目的:采用液相-固相萃取-超高效液相色谱-电喷雾串联质谱联用技术对27种色素建立了准确、灵敏的分析方法。方法:针对脂溶性、酸性和碱性3类色素分别采用不同的制备方法、色谱条件和电喷雾极性,采用4种不同药用部位的代表性药材进行了方法学考察。结果:表明方法线性关系良好(r≥0. 997);脂溶性和碱性色素的检测限为0. 03～3. 87 ng/g,酸性色素为0. 003～1. 94μg/g;准确度和精密度分别为70%～105%和0. 9%～6. 8%;应用于25个品种80批样品的筛查。结论:所建方法可靠、高效、准确,适用于中药材复杂基质中不同种类色素的测定。
Objective: To develop a sensitive and accurate method combining liquid and solid phase extraction with ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry to analyze 27 dyes. Methods: Different preparations,chromatography conditions and polarity of ESI were applied for 3 categories of lipophilic,acidic and basic dyes respectively. Four species of herbs representing different parts of plant were selected for methodology observation. Results: The linear correlation coefficient was good( r ≥ 0. 997). The LODs of oil soluble and basic dyes were 0. 03 ～ 3. 87 ng/g and acid dyes were 0. 003 ～1. 94 μg/g respectively. The accuracies and precisions were 70% ～ 105% and 0. 9% ～ 6. 8% respectively. Conclusion: After detecting 80 samples of 25 species herbs,this method proved to be reliable,efficient and accurate in the detection of different kinds of dyes in the complex matrix of herbs.
Objective: To develop a sensitive and accurate method combining liquid and solid phase extraction with ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry to analyze 27 dyes. Methods: Different preparations,chromatography conditions and polarity of ESI were applied for 3 categories of lipophilic,acidic and basic dyes respectively. Four species of herbs representing different parts of plant were selected for methodology observation. Results: The linear correlation coefficient was good( r ≥ 0. 997). The LODs of oil soluble and basic dyes were 0. 03 ～ 3. 87 ng/g and acid dyes were 0. 003 ～1. 94 μg/g respectively. The accuracies and precisions were 70% ～ 105% and 0. 9% ～ 6. 8% respectively. Conclusion: After detecting 80 samples of 25 species herbs,this method proved to be reliable,efficient and accurate in the detection of different kinds of dyes in the complex matrix of herbs.
引文
[1]国家食品药品监督管理局.总局关于中药材及饮片专项抽验结果的通告(2017年第5号)[EB/OL].2017-01-12(2017-03-22)http://www.sda.gov.cn/WS01/CL1872/168503.html.
[2]国家食品药品监督管理局.总局关于54批中药饮片不合格的通告(2017年第21号)[EB/OL].2017-02-09(2017-03-22)http://www.sda.gov.cn/WS01/CL1872/169415.html.
[3]国家食品药品监督管理局.总局关于23批次中药饮片不合格的通告(2017年第33号)[EB/OL].2017-02-23(2017-03-22)http://www.sda.gov.cn/WS01/CL1872/169865.html.
[4]Rafii F,Hall JD,Cerniglia CE.Mutagenicity of azo dyes used in foods,drugs and cosmetics before and after reduction by Clostridium species from the human intestinal tract[J].Food and Chemical Toxicology,1997,35:897-901.
[5]Nagaraja TN,Desiraju T.Effects of chronic consumption of metanil yellow by developing and adult rats on brain regional levels of noradrenaline,dopamine and serotonin,on acetylcholine esterase activity and on operantconditioning[J].Food and Chemical Toxicology,1993,31:41-44.
[6]Mpountoukas P,Pantazaki A,Kostareli E,Christodoulou P,Kareli D,Poliliou S.Cytogenetic evaluation and DNA interaction studies of the food colorants amaranth,erythrosine and tartrazine[J].Food and Chemical Toxicology,2010,48:2934-2944.
[7]Golka K,Kopps S,Myslak ZW.Carcinogenicity of azo colorants:influence of solubility and bioavailability[J].Toxicology Letters,2004,151:203-210.
[8]Gerasimov AV.Use of computers for processing thin-layer chromatograms based on an example of red food dyes[J].Vopr Pitan,2000,69(1-2):63-65.
[9]Markéta R,Petr T,Patrik V,Pavel K,Jan P.Sensitive determination of erythrosine and other red food colorants using capillary electrophoresis with laser-induced fluorescence detection[J].Journal of Chromatography A,2007,1141:206-211.
[10]Chen QC,Mou SF,Hou XP,Riviello JM,Ni ZM.Determination of eight synthetic food colorants in drinks by high-performance ion chromatography[J].Journal of Chromatography A.1998,827:73-81.
[11]刘敏,李小林,别玮,等.固相萃取-高效液相色谱法同时测定调味品中15种工业合成染料[J].色谱,2011,29(2):162-167.
[12]Yoshioka N,Ichihashi K.Determination of 40 synthetic food colors in drinks and candies by high-performance liquid chromatography using a short column with photodiode array detection[J].Talanta,2008,74(5):1408-1413.
[13]林维宣,孙兴权,赵雪蓉,等.高效液相色谱-串联质谱法同时检测化妆品中6种禁用着色剂[J].色谱,2012,30(5):527-532.
[14]Feng F,Zhao Y,Yong W,Sun L,Jiang G,Chu X.Highly sensitive and accurate screening of 40 dyes in soft drinks by liquid chromatography-electrospray tandem mass spectrometry[J].J Chromatogr BAnalyt Technol Biomed Life Sci,2011,879(20):1813-1818.
[15]张东雷,汪丽娜,陈小珍,等.超快速液相色谱-离子阱飞行时间质谱法测定肉制品中10种碱性染料[J].色谱,2012,30(8):770-776.
[16]赵延胜,杨敏莉,张峰,等.液相色谱/四极杆-飞行时间质谱法筛查奶酪中29种禁用和限用合成色素[J].色谱,2011,29(7):631-636.
[17]Jian S,Rui F,Qing H,Hong Y,Su Z,Lin F,et al.Simultaneous determination of sixteen synthetic acid pigments in medicinal Chinese herbs by polyamide SPE-HPLC[J].Chinese Traditional Patent Medicine,2015,37:1031-1036.
[18]Hu Q,Sun J,Yu H,Zhang S,Feng R,Ji S.Qualitative analysis of 50pigments in dyed herb by UHPLC/QTOF[J].Chinese Pharmaceutical Journal,2016,51(15):1316-1323.
[19]Li XQ,Zhang QH,Ma K,Li HM,Guo Z.Identification and determination of 34 water-soluble synthetic dyes in foodstuff by high performance liquid chromatography-diode array detection-ion trap timeof-flight tandem mass spectrometry[J].Food Chem,2015,182:316-326.
[20]冯月超,贾丽,何亚荟,等.超高效液相色谱-串联质谱法同时测定粮食及肉制品中的24种工业染料[J].色谱,2013,31(10):1021-1027.
[21]尹峰,丁召伟,杨志坚.固相萃取-高效液相色谱-串联质谱法检测香辛料中罗丹明B[J].色谱,2012,30(7):672-676.
[2]国家食品药品监督管理局.总局关于54批中药饮片不合格的通告(2017年第21号)[EB/OL].2017-02-09(2017-03-22)http://www.sda.gov.cn/WS01/CL1872/169415.html.
[3]国家食品药品监督管理局.总局关于23批次中药饮片不合格的通告(2017年第33号)[EB/OL].2017-02-23(2017-03-22)http://www.sda.gov.cn/WS01/CL1872/169865.html.
[4]Rafii F,Hall JD,Cerniglia CE.Mutagenicity of azo dyes used in foods,drugs and cosmetics before and after reduction by Clostridium species from the human intestinal tract[J].Food and Chemical Toxicology,1997,35:897-901.
[5]Nagaraja TN,Desiraju T.Effects of chronic consumption of metanil yellow by developing and adult rats on brain regional levels of noradrenaline,dopamine and serotonin,on acetylcholine esterase activity and on operantconditioning[J].Food and Chemical Toxicology,1993,31:41-44.
[6]Mpountoukas P,Pantazaki A,Kostareli E,Christodoulou P,Kareli D,Poliliou S.Cytogenetic evaluation and DNA interaction studies of the food colorants amaranth,erythrosine and tartrazine[J].Food and Chemical Toxicology,2010,48:2934-2944.
[7]Golka K,Kopps S,Myslak ZW.Carcinogenicity of azo colorants:influence of solubility and bioavailability[J].Toxicology Letters,2004,151:203-210.
[8]Gerasimov AV.Use of computers for processing thin-layer chromatograms based on an example of red food dyes[J].Vopr Pitan,2000,69(1-2):63-65.
[9]Markéta R,Petr T,Patrik V,Pavel K,Jan P.Sensitive determination of erythrosine and other red food colorants using capillary electrophoresis with laser-induced fluorescence detection[J].Journal of Chromatography A,2007,1141:206-211.
[10]Chen QC,Mou SF,Hou XP,Riviello JM,Ni ZM.Determination of eight synthetic food colorants in drinks by high-performance ion chromatography[J].Journal of Chromatography A.1998,827:73-81.
[11]刘敏,李小林,别玮,等.固相萃取-高效液相色谱法同时测定调味品中15种工业合成染料[J].色谱,2011,29(2):162-167.
[12]Yoshioka N,Ichihashi K.Determination of 40 synthetic food colors in drinks and candies by high-performance liquid chromatography using a short column with photodiode array detection[J].Talanta,2008,74(5):1408-1413.
[13]林维宣,孙兴权,赵雪蓉,等.高效液相色谱-串联质谱法同时检测化妆品中6种禁用着色剂[J].色谱,2012,30(5):527-532.
[14]Feng F,Zhao Y,Yong W,Sun L,Jiang G,Chu X.Highly sensitive and accurate screening of 40 dyes in soft drinks by liquid chromatography-electrospray tandem mass spectrometry[J].J Chromatogr BAnalyt Technol Biomed Life Sci,2011,879(20):1813-1818.
[15]张东雷,汪丽娜,陈小珍,等.超快速液相色谱-离子阱飞行时间质谱法测定肉制品中10种碱性染料[J].色谱,2012,30(8):770-776.
[16]赵延胜,杨敏莉,张峰,等.液相色谱/四极杆-飞行时间质谱法筛查奶酪中29种禁用和限用合成色素[J].色谱,2011,29(7):631-636.
[17]Jian S,Rui F,Qing H,Hong Y,Su Z,Lin F,et al.Simultaneous determination of sixteen synthetic acid pigments in medicinal Chinese herbs by polyamide SPE-HPLC[J].Chinese Traditional Patent Medicine,2015,37:1031-1036.
[18]Hu Q,Sun J,Yu H,Zhang S,Feng R,Ji S.Qualitative analysis of 50pigments in dyed herb by UHPLC/QTOF[J].Chinese Pharmaceutical Journal,2016,51(15):1316-1323.
[19]Li XQ,Zhang QH,Ma K,Li HM,Guo Z.Identification and determination of 34 water-soluble synthetic dyes in foodstuff by high performance liquid chromatography-diode array detection-ion trap timeof-flight tandem mass spectrometry[J].Food Chem,2015,182:316-326.
[20]冯月超,贾丽,何亚荟,等.超高效液相色谱-串联质谱法同时测定粮食及肉制品中的24种工业染料[J].色谱,2013,31(10):1021-1027.
[21]尹峰,丁召伟,杨志坚.固相萃取-高效液相色谱-串联质谱法检测香辛料中罗丹明B[J].色谱,2012,30(7):672-676.