超高效液相色谱-串联质谱法测定禽蛋中苏丹红的残留量
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摘要
目的建立禽蛋中苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ染料残留的液相色谱-串联质谱的检测方法。方法禽蛋样品中的苏丹红经溶解、冷冻离心及过滤提取纯化,经ZorbaxSB-C_(18)(2.1 mm×50 mm, 3.5μm)色谱柱,以乙腈和0.2%的甲酸水溶液为流动相进行等度洗脱,温度为35℃,流速为0.2mL/min,外标法定量。结果在1～50μg/kg的浓度范围内,线性关系良好(r>0.99),样品中的检出限0.5μg/kg,分析时间仅为5 min,加标回收率为69.5%～108.2%,相对标准偏差为1.6%～17.5%。结论该方法准确、快速、灵敏度高,适用于禽蛋中苏丹红染料的测定。
Objective To establish a method for determination of Sudan red Ⅰ, Ⅱ, Ⅲ and Ⅳ dye residues in poultry eggs by liquid chromatography-tandem mass spectrometry. Methods Sudan red was extracted and purified by dissolution, freezing centrifugation and filtration, then the samples were separated with a ZorbaxSB-C_(18)(2.1 mm×50 mm, 3.5 μm) column at the flow rate of 0.2 mL/min by isocratic elution using acetonitrile and 0.2% formic acid aqueous solution, the temperarure was maintained at 35 ℃, and quantified by external standard method. Result In the concentration range of 1-50 μg/kg, the linear relationship was good(r>0.99), the detection limit in the sample was 0.5 μg/kg, and the analysis time was only 5 min, and the standard recoveries were 69.5%-108.2%, the relative standard deviation were 1.6%-17.5%. Conclusion The method is accurate, rapid and sensitive, which is suitable for the determination of Sudan red dye in poultry eggs.
Objective To establish a method for determination of Sudan red Ⅰ, Ⅱ, Ⅲ and Ⅳ dye residues in poultry eggs by liquid chromatography-tandem mass spectrometry. Methods Sudan red was extracted and purified by dissolution, freezing centrifugation and filtration, then the samples were separated with a ZorbaxSB-C_(18)(2.1 mm×50 mm, 3.5 μm) column at the flow rate of 0.2 mL/min by isocratic elution using acetonitrile and 0.2% formic acid aqueous solution, the temperarure was maintained at 35 ℃, and quantified by external standard method. Result In the concentration range of 1-50 μg/kg, the linear relationship was good(r>0.99), the detection limit in the sample was 0.5 μg/kg, and the analysis time was only 5 min, and the standard recoveries were 69.5%-108.2%, the relative standard deviation were 1.6%-17.5%. Conclusion The method is accurate, rapid and sensitive, which is suitable for the determination of Sudan red dye in poultry eggs.
引文
[1]季宇彬,汲晨锋,高世勇,等.苏丹红Ⅰ、Ⅲ和Ⅳ对HepG-2细胞和SGC-7901细胞增殖的影响[J].环境科学,2006,27(6):1201-1207.Ji YB,Ji CF,Gao SY,et al.Effects of Sudan Red I,III and IV on the proliferation of HepG-2 cells and SGC-7901 cells[J].Environ Sci,2006,27(6):1201-1207.
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[8]徐秋生,刘俊厉,晨皓,等.凝胶渗透色谱-高效液相色谱法测定糟蛋中4种苏丹红的残留量[J].食品安全质量检测学报,2016,7(4):1694-1699.Xu QS,Liu JL,Chen H,et al.Detection of 4 kinds of Sudan Red dyes residues in wine cued egg by gel permeation chromatography-high performance liquid chromatography[J].J Food Saf Qual,2016,7(4):1694-1699.
[9]王春民,张秋萍,丁建森,等.食品中苏丹红的液相色谱三重串联四极杆质谱确认分析[J].上海预防医学杂志,2007,(10):501-503.Wang CM,Zhang QP,Ding JS,et al.Confirmation and analysis of Sudan Red in food by high performance liquid chromatography triple tandem quadrupole mass spectrometry[J].Shanghai J Prev Med,2007,(10):501-503.
[10]詹克航,时连.SPE-HPLC法测定辣椒及其制品中苏丹红色素含量[J].中国卫生检验杂志,2015,25(8):1169-1172.Zhan KH,Shi L.Detection of Sudan Red colorants in chili and pepper-based products by SPE-HPLC[J].Chin J Health Lab Technol,2015,25(8):1169-1172.
[11]党荣理,任立松,柳增善,等.食品中苏丹红I间接竞争ELISA方法的研究[J].中国食品卫生杂志,2010,22(4):336-339.Dang RL,Ren LS,Liu ZS,et al.Rapid ELISA for the detection of Sudan in foods[J].Chin J Food Hyg,2010,22(4):336-339.
[12]庞艳玲.食品中苏丹红检测方法的研究进展[J].食品与发酵工业,2008,34(3):115-119.Pang YL.Development in the analysis methods of Sudan Red in food[J].Food Ferment Ind,2008,34(3):115-119.
[13]夏宏宇,代正忙.苏丹红的毒性机理及检测[J].安庆师范学院学报,2005,(4):53-54.Xia HY,Dai ZM.The poison mechanism and calibaration method of Sudan[J].J Anqing Teach Colle(Nat Sci Ed),2005,(4):53-54.
[14]邱英莲.高效液相色谱法测定食品中的苏丹红[J].价值工程,2015,(23):164-165.Qiu YL.To determination Sudan Red in food by high performance liquid chromatography[J].Value Eng,2015,(23):164-165.
[15]冯华,王样培,王世俊,等.辣椒粉中非法添加苏丹红色素快速检验分析[J].食品安全质量检测学报,2018,9(13):3421-3426.Feng H,Wang YP,Wang SJ,et al.Rapid test and analysis of Sudan red illegally added into capsicum annuum[J].J Food Saf Qual,2018,9(13):3421-3426.
[16]陈美娟.致敏性分散染料和苏丹红染料的高效液相色谱及液质联用分析方法的研究[D].大连:大连理工大学,2006.Chen MJ.Study on the analytical methods of allergenic disperse dyes and sudan dyes by HPLC and LC-MS[D].Dalian:Dalian University of Technology,2006.
[17]王鹏,郭少飞,荆涛,等.基质固相分散液相色谱串联质谱法检测禽蛋中的苏丹红[J].色谱,2008,(3):353-357.Wang P,Guo SF,Jing T,et al.Determ ination of Sudan Red dyes in eggs using liquid chromatography tandem m ass spectrom etry and m atrix solid phase dispersion techn ique[J].Chin J Chromatogr,2008,(3):353-357.
[18]郝家勇,陈霞,李红敏,等.超高效液相色谱-电喷雾串联四极杆质谱法测定辣椒制品中的4中苏丹红[J].现代食品科技,2014,30(11):235-240.Hao JY,Chen X,Li MH,et al.Determination of four Sudan dyes in chilioducts using ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry[J].Mod Food Sci Technol,2014,30(11):235-240.
[19]王春民,张秋萍,丁建森,等.食品中苏丹红的液相色谱三重串联四极杆质谱确认分析[J].上海预防医学杂志,2007,19(10):501-503.Wang CM,Zhang QP,Ding JS,et al.Confirmation and analysis of Sudan Red in food by high performance liquid chromatography triple tandem quadrupole mass spectrometry[J].Shanghai J Preve Med,2007,19(10):501-503.
[2]Calbiani F,Careri M,Elviri L,et al.Accurate mass measurements for the confirmation of Sudan azo-dyes in hot chilli products by capillary liquid chromatography-electrospray tandem quadrupole orthogonal-acceleration time of flight mass spectrometry[J].J Chromatogr A,2004,(1058):127-135.
[3]韩爱云,左晓磊,霍惠玲,等.苏丹红事件及其毒性研究概况[J].福建农业,2015,(4):176-177.Han AY,Zuo XL,Huo HL,et al.Sudan Red incident and its toxicity[J].Fujian Agric,2015,(4):176-177.
[4]韩爱云,左晓磊,霍惠玲,等.食品中苏丹红残留检测研究进展[J].吉林农业,2015,14:69.Han AY,Zuo XL,Huo HL,et al.Research progress in detection of Sudan Red residues in food[J].Jili Agric,2015,(14):69.
[5]杨林飞,丁愈,张桂华,等.薄层色谱法检测食品中的苏丹红[J].实用预防医学,2006,13(1):185-186.Yang LF,Ding Y,Zhang GH,et al.Fast detection of Sudan Red by thin layer chromatography[J].Pract Prev Med,2006,13(1):185-186.
[6]吴银良,李存,刘勇军,等.高效液相色谱法快速测定鸭肉和鸭蛋中苏丹红染料[J].分析化学,2008,36(6):843-845.Wu YL,Li C,Liu YJ,et al.Fast determination of Sudan Dyes in duck meat and egg by high performance liquid chromatograhpy[J].Chin J Anal Chem,2008,36(6):843-845.
[7]苗崔.高效液相色谱法测定禽蛋中苏丹红残留量[J].现代食品,2018,(16):124-126.Miao C.Determination of Sudan Red residues in eggs by high performance liquid chromatography[J].Mod Food,2018,(16):124-126.
[8]徐秋生,刘俊厉,晨皓,等.凝胶渗透色谱-高效液相色谱法测定糟蛋中4种苏丹红的残留量[J].食品安全质量检测学报,2016,7(4):1694-1699.Xu QS,Liu JL,Chen H,et al.Detection of 4 kinds of Sudan Red dyes residues in wine cued egg by gel permeation chromatography-high performance liquid chromatography[J].J Food Saf Qual,2016,7(4):1694-1699.
[9]王春民,张秋萍,丁建森,等.食品中苏丹红的液相色谱三重串联四极杆质谱确认分析[J].上海预防医学杂志,2007,(10):501-503.Wang CM,Zhang QP,Ding JS,et al.Confirmation and analysis of Sudan Red in food by high performance liquid chromatography triple tandem quadrupole mass spectrometry[J].Shanghai J Prev Med,2007,(10):501-503.
[10]詹克航,时连.SPE-HPLC法测定辣椒及其制品中苏丹红色素含量[J].中国卫生检验杂志,2015,25(8):1169-1172.Zhan KH,Shi L.Detection of Sudan Red colorants in chili and pepper-based products by SPE-HPLC[J].Chin J Health Lab Technol,2015,25(8):1169-1172.
[11]党荣理,任立松,柳增善,等.食品中苏丹红I间接竞争ELISA方法的研究[J].中国食品卫生杂志,2010,22(4):336-339.Dang RL,Ren LS,Liu ZS,et al.Rapid ELISA for the detection of Sudan in foods[J].Chin J Food Hyg,2010,22(4):336-339.
[12]庞艳玲.食品中苏丹红检测方法的研究进展[J].食品与发酵工业,2008,34(3):115-119.Pang YL.Development in the analysis methods of Sudan Red in food[J].Food Ferment Ind,2008,34(3):115-119.
[13]夏宏宇,代正忙.苏丹红的毒性机理及检测[J].安庆师范学院学报,2005,(4):53-54.Xia HY,Dai ZM.The poison mechanism and calibaration method of Sudan[J].J Anqing Teach Colle(Nat Sci Ed),2005,(4):53-54.
[14]邱英莲.高效液相色谱法测定食品中的苏丹红[J].价值工程,2015,(23):164-165.Qiu YL.To determination Sudan Red in food by high performance liquid chromatography[J].Value Eng,2015,(23):164-165.
[15]冯华,王样培,王世俊,等.辣椒粉中非法添加苏丹红色素快速检验分析[J].食品安全质量检测学报,2018,9(13):3421-3426.Feng H,Wang YP,Wang SJ,et al.Rapid test and analysis of Sudan red illegally added into capsicum annuum[J].J Food Saf Qual,2018,9(13):3421-3426.
[16]陈美娟.致敏性分散染料和苏丹红染料的高效液相色谱及液质联用分析方法的研究[D].大连:大连理工大学,2006.Chen MJ.Study on the analytical methods of allergenic disperse dyes and sudan dyes by HPLC and LC-MS[D].Dalian:Dalian University of Technology,2006.
[17]王鹏,郭少飞,荆涛,等.基质固相分散液相色谱串联质谱法检测禽蛋中的苏丹红[J].色谱,2008,(3):353-357.Wang P,Guo SF,Jing T,et al.Determ ination of Sudan Red dyes in eggs using liquid chromatography tandem m ass spectrom etry and m atrix solid phase dispersion techn ique[J].Chin J Chromatogr,2008,(3):353-357.
[18]郝家勇,陈霞,李红敏,等.超高效液相色谱-电喷雾串联四极杆质谱法测定辣椒制品中的4中苏丹红[J].现代食品科技,2014,30(11):235-240.Hao JY,Chen X,Li MH,et al.Determination of four Sudan dyes in chilioducts using ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry[J].Mod Food Sci Technol,2014,30(11):235-240.
[19]王春民,张秋萍,丁建森,等.食品中苏丹红的液相色谱三重串联四极杆质谱确认分析[J].上海预防医学杂志,2007,19(10):501-503.Wang CM,Zhang QP,Ding JS,et al.Confirmation and analysis of Sudan Red in food by high performance liquid chromatography triple tandem quadrupole mass spectrometry[J].Shanghai J Preve Med,2007,19(10):501-503.
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