超高效液相色谱-串联质谱法测定食品中柑橘红2号和苏丹红Ⅰ～Ⅳ染料
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摘要
建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定食品中柑橘红2号和苏丹红Ⅰ～Ⅳ染料的检测方法。样品采用乙腈-氯化钠体系提取,NH2固相萃取柱净化,经超高效液相色谱分离,以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,三重四极杆质谱电喷雾电离(ESI+)检测,多反应监测模式(MRM),基质外标法定量。结果表明,柑橘红2号和苏丹红Ⅰ～Ⅳ5种成分在2～40 ng/m L范围内线性关系良好,决定系数(R~2)为0.998。低中高三个添加水平下,5种染料加标回收率在80.7%～114%之间,相对标准偏差范围<8.6%。方法检出限(S/N≥3)为5.0μg/kg,定量限(S/N≥10)为10.0μg/kg。该方法简便、快捷、高效、灵敏度高,适用于柑橘类水果、蜜饯、辣椒油、火锅底料及肉制品等多种食品基质中柑橘红2号和苏丹红Ⅰ～Ⅳ染料的同时检测。
A method for determination of Citrus Red 2 and SudanⅠ～ Ⅳ in food by ultra performance liquid chromatographytandem mass spectrometry was established.The samples were extracted with acetonitrile sodium chloride system and purified by NH2 column.The separation was carried out by ultra performance liquid chromatography( UPLC). The target compounds were detected by MS/MS system with electrospray ionization( ESI) under multiple reaction monitoring( MRM) mode.Results showed that,the calibration curves of 5 illegal dyes showed good linearity in 2 ～ 40 ng/m L with determination coefficients 0.998. The average recoveries ranged from 80.7% to 114% at three spiking levels with RSD < 8.6%.The limit of detection( LOD) and the limit of quantitation( LOQ) of Citrus Red 2 and SudanⅠ～ Ⅳ in five matrics were 5.0 and 10.0 μg/kg,respectively. This rapid and sensitive method could be applied for quantitative determination of Citrus Red 2 and SudanⅠ～ Ⅳ in foodstuff.
A method for determination of Citrus Red 2 and SudanⅠ～ Ⅳ in food by ultra performance liquid chromatographytandem mass spectrometry was established.The samples were extracted with acetonitrile sodium chloride system and purified by NH2 column.The separation was carried out by ultra performance liquid chromatography( UPLC). The target compounds were detected by MS/MS system with electrospray ionization( ESI) under multiple reaction monitoring( MRM) mode.Results showed that,the calibration curves of 5 illegal dyes showed good linearity in 2 ～ 40 ng/m L with determination coefficients 0.998. The average recoveries ranged from 80.7% to 114% at three spiking levels with RSD < 8.6%.The limit of detection( LOD) and the limit of quantitation( LOQ) of Citrus Red 2 and SudanⅠ～ Ⅳ in five matrics were 5.0 and 10.0 μg/kg,respectively. This rapid and sensitive method could be applied for quantitative determination of Citrus Red 2 and SudanⅠ～ Ⅳ in foodstuff.
引文
[1]鄢兵,张云伟,胡海山,等.高效液相色谱法测定食品中禁用物质碱性橙染料[J].理化检验-化学分册,2015,51(6):807-809.
[2]奚星林,王岚,李荀,等.HPLC-DAD法同时测定高脂肪食品中黄色2G、奶油黄、柑橘红2和苏丹红Ⅰ~Ⅳ[J].食品安全质量检测学报,2013,4(1):245-250.
[3]胡莉,雷绍荣,郭灵安.超高效液相色谱-串联质谱法测定脐橙中橘红2号染料[J].色谱,2012,30(8):832-835.
[4]R Rebane,I Leito,S Yurchenko,K Herodes. A review of analytical techniques for determination of Sudan I-IV dyes in food matrixes[J]. Journal of Chromatography A,2010,1217(17):2747-2757.
[5]陈毓芳,林海丹,李为鹏,等.高效液相色谱法测定果汁和果蔬中柑橘红2号染料[J].理化检验-化学分册,2011,47(5):536-538.
[6]黄晓兰,吴惠勤,黄芳,等.GC-MS/SIM法同时测定食品中苏丹红Ⅰ~Ⅳ[J].分析测试学报,2005,24(4):1-5.
[7]B Chen,Y Huang. Dispersive liquid-phase microextraction with solidification of floating organic droplet coupled with highperformance liquid chromatography for the determination of Sudan dyes in foodstuffs and water samples[J]. Journal of Agricultural and Food chemistry,2014,62(25):5818-5826.
[8]胡莉,仲伶俐,郭灵安,等.高压液相色谱法测定柑橘类水果中的柑橘红2号染料[J].食品安全质量检测学报,2013,4(5):1473-1477.
[9]吉林省卫生计生委.DBS22/017-2013食品安全地方标准柑橘类水果及其饮料中橘红2号的测定高效液相色谱法[S].北京:中国标准出版社,2013.
[10]四川省质监局.DB51/T 1883-2014柑橘中橘红2号染料的测定高效液相色谱法[S].北京:中国标准出版社,2014.
[11]F. Calbiani,M. Careri,L. Elviri,et al. Development and inhouse validation of a liquid chromatography-electrospray-tandem mass spectrometry method for the simultaneous determination of Sudan I,Sudan II,Sudan III and Sudan IV in hot chilli products[J].Journal of Chromatography A,2004,1042(1):123-130.
[12]毛江胜,王剑,孟静静,等.超高效液相色谱-电喷雾串联四级杆质谱法分析辣椒中的苏丹红染料[J].分析试验室(增刊),2009(28):341-344.
[13]刘正才,杨方,尹太坤,等.固相萃取/超高效液相色谱-串联质谱法同时测定禽蛋中4种苏丹红染料残留量[J].分析测试学报,2015,34(2):171-176.
[14]赵珊,张晶,丁晓静,等.凝胶净化/超高效液相色谱电喷雾质谱法检测调味油中11种禁用偶氮染料及罗丹明B[J].分析测试学报,2012,31(4):448-452.
[15]喻凌寒,杨运云,闫世平,等.高效液相色谱-离子阱质谱联用测定食品中的7种苏丹红染料[J].分析测试学报,2005,24(4):28-31.
[16]郝家勇,陈霞,李红敏,等.超高效液相色谱-串联四级杆质谱法测定辣椒制品中的4种苏丹红[J].现代食品科技,2014,30(11):235-240.
[17]马育松,艾连峰,李玮,等.凝胶净化/高效液相色谱-串联质谱法检测辣椒制品及肉制品中多种脂溶性着色剂[J].分析试验室,2014,33(2):195-200.
[18]吴坤.食品中柑橘红2号与罗丹明B及苏丹红Ⅰ~Ⅳ的高效液相色谱检验方法[J].农产品加工(学刊),2014,10(10):67-68.
[19]李玮,艾连峰,魏欣欣,等.高效液相色谱-二极管阵列检测法同时测定糖果中11种脂溶性着色剂[J].分析科学学报,2015,31(6):820-824.
[20]马育松,李玮,艾连峰,等.高效液相色谱/二极管阵列检测器同时测定辣椒及其制品中11种脂溶性着色剂[J].分析测试学报,2014,33(1):93-97.
[2]奚星林,王岚,李荀,等.HPLC-DAD法同时测定高脂肪食品中黄色2G、奶油黄、柑橘红2和苏丹红Ⅰ~Ⅳ[J].食品安全质量检测学报,2013,4(1):245-250.
[3]胡莉,雷绍荣,郭灵安.超高效液相色谱-串联质谱法测定脐橙中橘红2号染料[J].色谱,2012,30(8):832-835.
[4]R Rebane,I Leito,S Yurchenko,K Herodes. A review of analytical techniques for determination of Sudan I-IV dyes in food matrixes[J]. Journal of Chromatography A,2010,1217(17):2747-2757.
[5]陈毓芳,林海丹,李为鹏,等.高效液相色谱法测定果汁和果蔬中柑橘红2号染料[J].理化检验-化学分册,2011,47(5):536-538.
[6]黄晓兰,吴惠勤,黄芳,等.GC-MS/SIM法同时测定食品中苏丹红Ⅰ~Ⅳ[J].分析测试学报,2005,24(4):1-5.
[7]B Chen,Y Huang. Dispersive liquid-phase microextraction with solidification of floating organic droplet coupled with highperformance liquid chromatography for the determination of Sudan dyes in foodstuffs and water samples[J]. Journal of Agricultural and Food chemistry,2014,62(25):5818-5826.
[8]胡莉,仲伶俐,郭灵安,等.高压液相色谱法测定柑橘类水果中的柑橘红2号染料[J].食品安全质量检测学报,2013,4(5):1473-1477.
[9]吉林省卫生计生委.DBS22/017-2013食品安全地方标准柑橘类水果及其饮料中橘红2号的测定高效液相色谱法[S].北京:中国标准出版社,2013.
[10]四川省质监局.DB51/T 1883-2014柑橘中橘红2号染料的测定高效液相色谱法[S].北京:中国标准出版社,2014.
[11]F. Calbiani,M. Careri,L. Elviri,et al. Development and inhouse validation of a liquid chromatography-electrospray-tandem mass spectrometry method for the simultaneous determination of Sudan I,Sudan II,Sudan III and Sudan IV in hot chilli products[J].Journal of Chromatography A,2004,1042(1):123-130.
[12]毛江胜,王剑,孟静静,等.超高效液相色谱-电喷雾串联四级杆质谱法分析辣椒中的苏丹红染料[J].分析试验室(增刊),2009(28):341-344.
[13]刘正才,杨方,尹太坤,等.固相萃取/超高效液相色谱-串联质谱法同时测定禽蛋中4种苏丹红染料残留量[J].分析测试学报,2015,34(2):171-176.
[14]赵珊,张晶,丁晓静,等.凝胶净化/超高效液相色谱电喷雾质谱法检测调味油中11种禁用偶氮染料及罗丹明B[J].分析测试学报,2012,31(4):448-452.
[15]喻凌寒,杨运云,闫世平,等.高效液相色谱-离子阱质谱联用测定食品中的7种苏丹红染料[J].分析测试学报,2005,24(4):28-31.
[16]郝家勇,陈霞,李红敏,等.超高效液相色谱-串联四级杆质谱法测定辣椒制品中的4种苏丹红[J].现代食品科技,2014,30(11):235-240.
[17]马育松,艾连峰,李玮,等.凝胶净化/高效液相色谱-串联质谱法检测辣椒制品及肉制品中多种脂溶性着色剂[J].分析试验室,2014,33(2):195-200.
[18]吴坤.食品中柑橘红2号与罗丹明B及苏丹红Ⅰ~Ⅳ的高效液相色谱检验方法[J].农产品加工(学刊),2014,10(10):67-68.
[19]李玮,艾连峰,魏欣欣,等.高效液相色谱-二极管阵列检测法同时测定糖果中11种脂溶性着色剂[J].分析科学学报,2015,31(6):820-824.
[20]马育松,李玮,艾连峰,等.高效液相色谱/二极管阵列检测器同时测定辣椒及其制品中11种脂溶性着色剂[J].分析测试学报,2014,33(1):93-97.