DART-Q-Orbitrap MS法快速检测豆制品中碱性橙Ⅱ和金胺O
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摘要
采用实时直接分析(direct analysis in real time,DART)离子化技术与四极杆-静电场轨道阱高分辨质谱联用技术(Q-Orbitrap MS),建立了快速定性和定量分析方法,检测豆制品中非法添加的碱性橙Ⅱ和金胺O。在正离子模式下,采用Full MS/targetrd-MS2扫描方式,可直接将豆制品置于离子化区域内对两种染料进行快速定性分析。在定量分析中,采用80%乙腈水溶液提取样品,应用Dip-it载样方式,对实验参数进行系统性优化。采用空白基质溶液进行梯度稀释,测得碱性橙Ⅱ和金胺O在基质中的检出限均为0.2mg/L;采用内标法定量,在1～20mg/L浓度范围内线性关系良好,相关系数分别为0.997 2和0.999 4。该方法快速准确,可为食品中非法添加染料的定性和定量检测提供参考依据。
A method of direct analysis in real time coupled with Orbitrap mass spectrometer was developed for the qualitative and quantitative analysis of Basic Orange Ⅱ and Auramine O in bean products.In qualitative analysis,the Full MS/Targeted MS2 mode was applied to obtain the mass spectrum,bean products could be directly analyzed in the ionized area.DART parameters were systematically optimized to achieve the best detection performance.The component was identified by comparing with standard component and the report of relative researches as well as the full scan spectra and secondary spectra.In quantitative analysis,simple liquid extracted by 80%acetonitrile without further clean-up was used for sample preparation.Dip-it sampler was used for automatic sampling.The two pigments were subjected to gradient dilution by blank matrix solution,and both the limits of detection are 0.2 mg/L,and the linear relation in the range of1-20 mg/L are well.The correlation coefficients are 0.997 2 and 0.999 4 for Basic OrangeⅡand Auramine O.The method is rapid and accurate,and can provide reference for the qualitative and quantitative addition of pigments in foods.
A method of direct analysis in real time coupled with Orbitrap mass spectrometer was developed for the qualitative and quantitative analysis of Basic Orange Ⅱ and Auramine O in bean products.In qualitative analysis,the Full MS/Targeted MS2 mode was applied to obtain the mass spectrum,bean products could be directly analyzed in the ionized area.DART parameters were systematically optimized to achieve the best detection performance.The component was identified by comparing with standard component and the report of relative researches as well as the full scan spectra and secondary spectra.In quantitative analysis,simple liquid extracted by 80%acetonitrile without further clean-up was used for sample preparation.Dip-it sampler was used for automatic sampling.The two pigments were subjected to gradient dilution by blank matrix solution,and both the limits of detection are 0.2 mg/L,and the linear relation in the range of1-20 mg/L are well.The correlation coefficients are 0.997 2 and 0.999 4 for Basic OrangeⅡand Auramine O.The method is rapid and accurate,and can provide reference for the qualitative and quantitative addition of pigments in foods.
引文
[1]许雪琴,刘琼华,杨方,钱疆,陈健林,振宇,邱彬.SERS活性基底的制备及其在腐竹中碱性橙Ⅱ的检测研究[J].光谱学与光谱分析,2015,35(11):3 092-3 095.XU Xueqin,LIU Qionghua,YANG Fang,QIAN Jiang,CHEN Jianlin,ZHEN Yu,QIUBin.Preparation of gold nano-particles as surface-enhanced raman scattering sensors for analysis of banned food dye chrysoidin in yuba[J].Spectroscopy and Spectral Analysis,2015,35(11):3 092-3 095(in Chinese).
[2]朱浩,李小平,陈晓红,金米聪.固相萃取-高效液相色谱法同时测定豆制品中的碱性嫩黄O、酸性橙Ⅱ和碱性橙Ⅱ[J].分析实验室,2013,32(9):63-67.ZHU Hao,LI Xiaoping,CHEN Xiaohong,JINMicong.Solid-phase extraction combined with high-performance liquid chromatographic method for simultaneous determination of auramine O,acid OrangeⅡand basic OrangeⅡin bean products[J].Chinese Journal of Analysis Laboratory,2013,32(9):63-67(in Chinese).
[3]FANG G,FENG J,YAN Y,LIU C,WANG S.Highly selective determination of chrysoidine in foods through a surface molecularly imprinted sol-gel polymer solid-phase extraction coupled with HPLC[J].Food Analytical Methods,2014,7(2):345-351.
[4]林黛琴,万承波,邱萍,刘花梅.液相色谱-串联质谱法快速测定食品中4种黄色工业染料[J].质谱学报,2013,34(3):170-178.LIN Daiqin,WAN Chengbo,QIU Ping,LIUHuamei.Rapid determination of four high yellow dyes in foods by HPLC-MS/MS[J].Journal of Chinese Mass Spectrometry Society,2013,34(3):170-178(in Chinese)
[5]赵珊,张晶,丁晓静,杨蕴嘉,邵兵.超高效液相色谱电喷雾串联四极杆质谱法检测豆制品中12种禁用工业染料[J].分析测试学报,2016,35(4):432-437.ZHAO Shan,ZHANG Jing,DING Xiaojing,YANG Yunjia,SHAO Bing.Determination of12banned dyes in soy products by ultra performance liquid chromatography with electospray ionization tandem mass spectrometry[J].Journal of Instrumental Analysis,2016,35(4):432-437(in Chinese).
[6]丁晓静,张晶,邵兵,赵珊.反相高效液相色谱法测定豆制品中碱性橙2[J].首都公共卫生,2017,(6):259-261.DING Xiaojing,ZHANG Jing,SHAO Bing,ZHAO Shan.Determination of chrysoidine in bean products by reversed phase high performance liquid chromatography[J].Capital Journal of Public Health,2017,(6):259-261(in Chinese).
[7]TAKATS Z,WISEMAN J M,GOLOGAN B,COOKS R G.Mass spectrometry sampling under ambient conditions with desorption electrospray ionization[J].Science,2004,306:471-473.
[8]张佳玲,霍飞凤,周志贵,白玉,刘虎威.实时直接分析质谱的原理及应用[J].化学进展,2012,24(1):101-109.ZHANG Jialing,HUO Feifeng,ZHOU Zhigui,BAI Yu,LIU Huwei.The principles and applications of an ambient ionization method-direct analysis in real time(DART)[J].Progress in Chemistry,2012,24(1):101-109(in Chinese).
[9]刘占芳,周红,孙振文,朱军,张冠男,乔婷,赵彦彪,徐建中.实时直接分析-飞行时间质谱新技术在微量物证检验中的应用[J].刑事技术,2017,42(2):147-150.LIU Zhanfang,ZHOU Hong,SUN Zhenwen,ZHU Jun,ZHANG Guannan,QIAO Ting,ZHAO Yanbiao,XU Jianzhong.The application of DART-TOFMS into trace evidence[J].Forensic Science and Technology,2017,42(2):147-150(in Chinese).
[10]王勇为,叶芳挺.Thermo Scientific Q Exactive台式四极杆-轨道阱高分辨质谱仪[J].中国食品,2011,590(22):64-65.WANG Yongwei,YE Fangting.Thermo Scientific Q-Exactive MS[J].China Food,2011,590(22):64-65(in Chinese).
[11]郭云龙,王洋,李波,高凤志,刘淑莹.DART-MS快速检测中药材中非法染色物质金胺O[J].分析试验室,2014,33(11):1 245-1 248.GUO Yunlong,WANG Yang,LI Bo,GAOFengzhi,LIU Shuying.Identification of illegal addition of auramine O in chinese medicine by direct analysis in real time mass spectrometry[J].Chinese Journal of Analysis Laboratory,2014,33(11):1 245-1 248(in Chinese).
[12]张百乐,高黎红,解迎双,周围,陈晓峰,雷春妮,张欢.实时直接分析-串联质谱法快速筛查火锅底料、牛肉面汤及调味料中罂粟壳生物碱[J].色谱,2017,35(7):724-729.ZHANG Baile,GAO Lihong,XIE Yingshuang,ZHOU Wei,CHEN Xiaofeng,LEI Chunni,ZHANG Huan.Rapid screening the alkaloids of poppy shell in hot pot condiment,beef noodle soup and seasoning by direct analysis in real timetandem mass spectrometry[J].Chinese Journal of Chromatography,2017,35(7):724-729(in Chinese).
[13]李乐乐,郭云龙,刘文龙,李卓,王洋,刘淑莹.DART-Orbitrap质谱法对黄芩药材的快速分析[J].分析测试学报,2016,35(7):859-863.LI Lele,GUO Yunlong,LIU Wenlong,LIZhuo,WANG Yang,LIU Shuying.Rapid analysis of Scutellaria Radix by using DART coupled with Orbitrap mass spectrometry[J].Journal of Instrumental Analysis,2016,35(7):859-863(in Chinese).
[14]GROSS J H.Direct analysis in real time-a critical review on DART-MS[J].Cheminform,2014,406(1):63-80.
[15]HIRAOKA K,NINOMIYA S,CHEN L C,IWAMA T,MANDAL M K,SUZUKI H,ARIYADA O,FURUYA H,TAKEKAWA K.Development of double cylindrical dielectric barrier discharge ion source[J].Analyst,2011,136:1 210-1 215.
[16]HARRIS G A,GALHENA A S,FERNANDEZF M.Ambient sampling/ionization mass spectrometry:applications and current trends[J].Analytical Chemistry,2011.82(13):4 508.
[17]李媛媛,王洋,刘斌,石金娥,王莹,王伟,张琳琳.高效液相色谱-串联质谱法快速测定腐竹中2种工业染料[J].吉林蔬菜,2014,(12):46-47.LI Yuanyuan,WANG Yang,LIU Bing,SHI Jiner,WANG Ying,WANG Wei,ZHANG Lingling.Determination of basic orangeⅡ、auramine O in Yuba using liquid chromatography-mass spectrometry[J].Jilin Vegetable,2014,(12):46-47(in Chinese).
[18]FENN J B,MANN M,MENG C K,WONG SF.Electrospray ionization-principles and practice[J].Mass Spectrometry Reviews,1990,9(1):37-70.
[19]TANAKA K,WAKI H,IDO Y,AKITA S,YOSHIDA Y,YOSHIDA T,MATSUO T.Protein and polymer analyses up to m/z 100 000by laser ionization time-of-flight mass spectrometry[J].Rapid Communications in Mass Spectrometry,1988,2(8):151-153.
[20]李中权,张芳,苏越,郭寅龙.质谱直接定量分析技术的应用进展[J].质谱学报,2018,39(2):129-140.LI Zhongquan,ZHANG Fang,SU Yue,GUOYinlong.Advances in direct quantification analysis by mass spectrometry[J].Journal of Chinese Mass Spectrometry Society,2018,39(2):129-140(in Chinese).
[21]CHEN D,HUANG Y Q,HE X M,SHI Z G,FENG Y Q.Coupling carbon nanotube film microextraction with desorption corona beam ionization for rapid analysis of Sudan dyes(Ⅰ-Ⅳ)and Rhodamine B in chilli oil[J].Analyst,2015,140(5):1 731-1 738.
[22]CUI M,MCCOOEYE M A,CATHARINEFRASER A.Quantitation of lysergic acid diethylamide in urine using atmospheric pressure matrix-assisted laser desorption/ionization ion trap mass spectrometry[J].Analytical Chemistry,2004,76(23):7 143-7 148.
[23]WISEMAN J M,EVANS C A,BOWEN C L,KENNEDY J H.Direct analysis of dried blood spots utilizing desorption electrospray ionization(DESI)mass spectrometry[J].Analyst,2010,135(4):720-725.
[24]张华,任盼盼,陈健,王礼治,贺含毅,欧阳永中,陈焕文.内部萃取电喷雾电离质谱法分析红辣椒[J].质谱学报,2015,36(5):411-416.ZHANG Hua,REN Panpan,CHEN Jian,WANG Lizhi,HE Hanyi,OUYANG Yongzhong,CHEN Huanwen.Direct analysis of red peppers using internal extractive electrospray ionization mass spectrometry[J].Journal of Chinese Mass Spectrometry Society,2015,36(5):411-416(in Chinese).
[2]朱浩,李小平,陈晓红,金米聪.固相萃取-高效液相色谱法同时测定豆制品中的碱性嫩黄O、酸性橙Ⅱ和碱性橙Ⅱ[J].分析实验室,2013,32(9):63-67.ZHU Hao,LI Xiaoping,CHEN Xiaohong,JINMicong.Solid-phase extraction combined with high-performance liquid chromatographic method for simultaneous determination of auramine O,acid OrangeⅡand basic OrangeⅡin bean products[J].Chinese Journal of Analysis Laboratory,2013,32(9):63-67(in Chinese).
[3]FANG G,FENG J,YAN Y,LIU C,WANG S.Highly selective determination of chrysoidine in foods through a surface molecularly imprinted sol-gel polymer solid-phase extraction coupled with HPLC[J].Food Analytical Methods,2014,7(2):345-351.
[4]林黛琴,万承波,邱萍,刘花梅.液相色谱-串联质谱法快速测定食品中4种黄色工业染料[J].质谱学报,2013,34(3):170-178.LIN Daiqin,WAN Chengbo,QIU Ping,LIUHuamei.Rapid determination of four high yellow dyes in foods by HPLC-MS/MS[J].Journal of Chinese Mass Spectrometry Society,2013,34(3):170-178(in Chinese)
[5]赵珊,张晶,丁晓静,杨蕴嘉,邵兵.超高效液相色谱电喷雾串联四极杆质谱法检测豆制品中12种禁用工业染料[J].分析测试学报,2016,35(4):432-437.ZHAO Shan,ZHANG Jing,DING Xiaojing,YANG Yunjia,SHAO Bing.Determination of12banned dyes in soy products by ultra performance liquid chromatography with electospray ionization tandem mass spectrometry[J].Journal of Instrumental Analysis,2016,35(4):432-437(in Chinese).
[6]丁晓静,张晶,邵兵,赵珊.反相高效液相色谱法测定豆制品中碱性橙2[J].首都公共卫生,2017,(6):259-261.DING Xiaojing,ZHANG Jing,SHAO Bing,ZHAO Shan.Determination of chrysoidine in bean products by reversed phase high performance liquid chromatography[J].Capital Journal of Public Health,2017,(6):259-261(in Chinese).
[7]TAKATS Z,WISEMAN J M,GOLOGAN B,COOKS R G.Mass spectrometry sampling under ambient conditions with desorption electrospray ionization[J].Science,2004,306:471-473.
[8]张佳玲,霍飞凤,周志贵,白玉,刘虎威.实时直接分析质谱的原理及应用[J].化学进展,2012,24(1):101-109.ZHANG Jialing,HUO Feifeng,ZHOU Zhigui,BAI Yu,LIU Huwei.The principles and applications of an ambient ionization method-direct analysis in real time(DART)[J].Progress in Chemistry,2012,24(1):101-109(in Chinese).
[9]刘占芳,周红,孙振文,朱军,张冠男,乔婷,赵彦彪,徐建中.实时直接分析-飞行时间质谱新技术在微量物证检验中的应用[J].刑事技术,2017,42(2):147-150.LIU Zhanfang,ZHOU Hong,SUN Zhenwen,ZHU Jun,ZHANG Guannan,QIAO Ting,ZHAO Yanbiao,XU Jianzhong.The application of DART-TOFMS into trace evidence[J].Forensic Science and Technology,2017,42(2):147-150(in Chinese).
[10]王勇为,叶芳挺.Thermo Scientific Q Exactive台式四极杆-轨道阱高分辨质谱仪[J].中国食品,2011,590(22):64-65.WANG Yongwei,YE Fangting.Thermo Scientific Q-Exactive MS[J].China Food,2011,590(22):64-65(in Chinese).
[11]郭云龙,王洋,李波,高凤志,刘淑莹.DART-MS快速检测中药材中非法染色物质金胺O[J].分析试验室,2014,33(11):1 245-1 248.GUO Yunlong,WANG Yang,LI Bo,GAOFengzhi,LIU Shuying.Identification of illegal addition of auramine O in chinese medicine by direct analysis in real time mass spectrometry[J].Chinese Journal of Analysis Laboratory,2014,33(11):1 245-1 248(in Chinese).
[12]张百乐,高黎红,解迎双,周围,陈晓峰,雷春妮,张欢.实时直接分析-串联质谱法快速筛查火锅底料、牛肉面汤及调味料中罂粟壳生物碱[J].色谱,2017,35(7):724-729.ZHANG Baile,GAO Lihong,XIE Yingshuang,ZHOU Wei,CHEN Xiaofeng,LEI Chunni,ZHANG Huan.Rapid screening the alkaloids of poppy shell in hot pot condiment,beef noodle soup and seasoning by direct analysis in real timetandem mass spectrometry[J].Chinese Journal of Chromatography,2017,35(7):724-729(in Chinese).
[13]李乐乐,郭云龙,刘文龙,李卓,王洋,刘淑莹.DART-Orbitrap质谱法对黄芩药材的快速分析[J].分析测试学报,2016,35(7):859-863.LI Lele,GUO Yunlong,LIU Wenlong,LIZhuo,WANG Yang,LIU Shuying.Rapid analysis of Scutellaria Radix by using DART coupled with Orbitrap mass spectrometry[J].Journal of Instrumental Analysis,2016,35(7):859-863(in Chinese).
[14]GROSS J H.Direct analysis in real time-a critical review on DART-MS[J].Cheminform,2014,406(1):63-80.
[15]HIRAOKA K,NINOMIYA S,CHEN L C,IWAMA T,MANDAL M K,SUZUKI H,ARIYADA O,FURUYA H,TAKEKAWA K.Development of double cylindrical dielectric barrier discharge ion source[J].Analyst,2011,136:1 210-1 215.
[16]HARRIS G A,GALHENA A S,FERNANDEZF M.Ambient sampling/ionization mass spectrometry:applications and current trends[J].Analytical Chemistry,2011.82(13):4 508.
[17]李媛媛,王洋,刘斌,石金娥,王莹,王伟,张琳琳.高效液相色谱-串联质谱法快速测定腐竹中2种工业染料[J].吉林蔬菜,2014,(12):46-47.LI Yuanyuan,WANG Yang,LIU Bing,SHI Jiner,WANG Ying,WANG Wei,ZHANG Lingling.Determination of basic orangeⅡ、auramine O in Yuba using liquid chromatography-mass spectrometry[J].Jilin Vegetable,2014,(12):46-47(in Chinese).
[18]FENN J B,MANN M,MENG C K,WONG SF.Electrospray ionization-principles and practice[J].Mass Spectrometry Reviews,1990,9(1):37-70.
[19]TANAKA K,WAKI H,IDO Y,AKITA S,YOSHIDA Y,YOSHIDA T,MATSUO T.Protein and polymer analyses up to m/z 100 000by laser ionization time-of-flight mass spectrometry[J].Rapid Communications in Mass Spectrometry,1988,2(8):151-153.
[20]李中权,张芳,苏越,郭寅龙.质谱直接定量分析技术的应用进展[J].质谱学报,2018,39(2):129-140.LI Zhongquan,ZHANG Fang,SU Yue,GUOYinlong.Advances in direct quantification analysis by mass spectrometry[J].Journal of Chinese Mass Spectrometry Society,2018,39(2):129-140(in Chinese).
[21]CHEN D,HUANG Y Q,HE X M,SHI Z G,FENG Y Q.Coupling carbon nanotube film microextraction with desorption corona beam ionization for rapid analysis of Sudan dyes(Ⅰ-Ⅳ)and Rhodamine B in chilli oil[J].Analyst,2015,140(5):1 731-1 738.
[22]CUI M,MCCOOEYE M A,CATHARINEFRASER A.Quantitation of lysergic acid diethylamide in urine using atmospheric pressure matrix-assisted laser desorption/ionization ion trap mass spectrometry[J].Analytical Chemistry,2004,76(23):7 143-7 148.
[23]WISEMAN J M,EVANS C A,BOWEN C L,KENNEDY J H.Direct analysis of dried blood spots utilizing desorption electrospray ionization(DESI)mass spectrometry[J].Analyst,2010,135(4):720-725.
[24]张华,任盼盼,陈健,王礼治,贺含毅,欧阳永中,陈焕文.内部萃取电喷雾电离质谱法分析红辣椒[J].质谱学报,2015,36(5):411-416.ZHANG Hua,REN Panpan,CHEN Jian,WANG Lizhi,HE Hanyi,OUYANG Yongzhong,CHEN Huanwen.Direct analysis of red peppers using internal extractive electrospray ionization mass spectrometry[J].Journal of Chinese Mass Spectrometry Society,2015,36(5):411-416(in Chinese).