改进固相萃取-高效液相色谱法同时测定食品中7种合成着色剂
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摘要
目的建立固相萃取-高效液相色谱法同时测定食品中7种合成着色剂(柠檬黄、日落黄、苋菜红、胭脂红、新红、赤藓红和亮蓝)的含量。方法使用Welchrom?PA聚酰胺固相萃取小柱和Welchrom?P-WAX弱阴离子交换固相萃取小柱对多种食品基质进行净化、浓缩,并采用Ultimate?XB-C18(250 mm×4.6 mm, 5μm)色谱柱以甲醇-0.02mol/L乙酸铵为流动相进行梯度洗脱,于254nm波长下测定。结果 Welchrom?PA聚酰胺小柱和Welchrom?P-WAX弱阴离子交换固相萃取小柱分别对固体和液体样品中杂质的去除效果好、回收率高。7种合成着色剂在浓度为0.5～50μg/mL的范围内线性关系良好(r2>0.9995),回收率为84.7%～105.8%,检出限为0.2～0.5 mg/kg。结论该方法简便、灵敏度高、准确性好,适用于食品中7种合成着色剂的定量分析。
Objective To establish a method for the simultaneous determination of 7 kinds of synthetic colorants(lemon yellow, sunset yellow, amaranth, carmine, new red, red oak and bright blue) by solid phase extraction-high performance liquid chromatography(HPLC). Methods Welchrom? PA polyamide solid-phase extraction column and Welchrom? P-WAX weak anion exchange solid-phase extraction column were used to purify and concentrate a variety of food matrix. The samples were separated with a Ultimate? XB-C18 colum(250 mm×4.6 mm, 5 μm) by gradient elution using methanol and 0.02 mol/L ammonium acetate as mobile phase, and detected at 254 nm wavelength. Results Welchrom? PA polyamide solid-phase extraction column and Welchrom? P-WAX weak anion exchange solid-phase extraction column had good removal of impurities and high recovery rates in solid and liquid samples, respectively. Seven kinds of synthetic colorants had good linear relations in the range of concentration of 0.5-50 g/mL(r2 >0.9995), the recovery rates were 84.7%-105.8%, and the limits of detection were 0.2-0.5 mg/kg. Conclusion This method is simple, sensitive and accurate, and it is suitable for quantitative analysis of 7 kinds of synthetic colorants in food.
Objective To establish a method for the simultaneous determination of 7 kinds of synthetic colorants(lemon yellow, sunset yellow, amaranth, carmine, new red, red oak and bright blue) by solid phase extraction-high performance liquid chromatography(HPLC). Methods Welchrom? PA polyamide solid-phase extraction column and Welchrom? P-WAX weak anion exchange solid-phase extraction column were used to purify and concentrate a variety of food matrix. The samples were separated with a Ultimate? XB-C18 colum(250 mm×4.6 mm, 5 μm) by gradient elution using methanol and 0.02 mol/L ammonium acetate as mobile phase, and detected at 254 nm wavelength. Results Welchrom? PA polyamide solid-phase extraction column and Welchrom? P-WAX weak anion exchange solid-phase extraction column had good removal of impurities and high recovery rates in solid and liquid samples, respectively. Seven kinds of synthetic colorants had good linear relations in the range of concentration of 0.5-50 g/mL(r2 >0.9995), the recovery rates were 84.7%-105.8%, and the limits of detection were 0.2-0.5 mg/kg. Conclusion This method is simple, sensitive and accurate, and it is suitable for quantitative analysis of 7 kinds of synthetic colorants in food.
引文
[1]奚星林,邵仕萍,徐娟,等.固相萃取高效液相色谱法同时测定食品中12种合成色素[J].中国食品卫生杂志,2012,24(3):217-222.Xi XL,Shao SP,Xu J,et al.Simultaneous determination of 12 synthetic colorants in foods with solid-phase extracted high performance liquid chromatography[J].Chin J Food Hyg,2012,24(3):217-222.
[2]刘谦,李熙,吴新欣,等.高效液相色谱法同时测定复杂食品基质中8种合成色素的含量[J].理化检验-化学分册,2017,53(6):693-696.Liu Q,Li X,Wu XX,et al.Simultaneous determination of 8 kinds of synthetic cpmplex food matrix by HPLC[J].Phys Test Chem Anal B,2017,53(6):693-696.
[3]陈彦凤,肖白曼,孙彦芳,等.固相萃取-高效液相色谱法测定肉制品中合成着色剂的含量[J].中国食品卫生杂志,2013,25(5):428-430.Chen YF,Xiao BM,Sun YF,et al.Determination of synthetic colorants in meat products by SPE-HPLC[J].Chin J Food Hyg,2013,25(5):428-430.
[4]赵延胜,董英,张峰,等.食品中46种禁限用合成色素的分级提取净化体系研究[J].分析化学,2012,40(2):249-256.Zhao YS,Dong Y,Zhang F,et al.A study on system of sequential extraction and cleaning of 46 forbidden and limited synthetic pigments in food stuff[J].Chin Anal Chem,2012,40(2):249-256.
[5]毕小玲,宋娟,庄晓洪,等.固相萃取-HPLC法检测熟肉制品中合成色素[J].食品研究与开发,2017,38(5):180-183.Bi XL,Song J,Zhuang XH,et al.Determination of synthetic pigments in cooked meat by solid phase extraction and HPLC[J].Food Res Dev,2017,38(5):180-183.
[6]邹志飞,蒲民,李建军,等.各国(地区)食用色素的使用现况与比对分析[J].中国食品卫生杂志,2010,22(2):112-121.Zou ZF,Pu M,Li JJ,et al.Usage status and comparison analysis of the food colour in some countries(regions)[J].Chin J Food Hyg,2010,22(2):112-121.
[7]林芳,李涛,王一欣,等.固相萃取-超高效液相色谱法同时测定蜜饯中9种合成色素[J].食品安全质量检测学报,2016,7(2):567-574.Lin F,Li T,Wang YX,et al.Simultaneous determination of 9 kinds of synthetic pigments in preserved fruit by solid phase sxtraction-ultra high performance liquid chromatography[J].J Food Saf Qual,2016,7(2):567-574.
[8]刘艳琴,王浩,杨红梅,等.固相萃取-HPLC法同时测定糕点中8种人工合成色素[J].食品研究与开发,2010,31(2):139-142.Liu YQ,Wang H,Yang HM,et al.Determination of 8 synthetic colours in cake by solid-phase extraction couple with high performance liquid chromatography[J].Food Res Dev,2010,31(2):139-142.
[9]GB 2760-2014食品安全国家标准食品添加剂使用标准[S].GB 2760-2014 National food safety standard-Standard for uses of food additives[S].
[10]杨桂君,高文惠.毛细管电泳法测定食品中8种添加剂[J].食品科学,2010,31(8):377-380.Yang GJ,Gao WH.Determination of eight food additives in different matrices by capillary electrophoresis[J].Food Sci,2010,31(8):377-380.
[11]王丽芳,丁晓静,解娜,等.毛细管电泳法测定糖果及调制酒中10种人工合成色素[J].食品科学,2014,35(14):145-150.Wang LF,Ding XJ,Xie N,et al.Simultaneous determination of ten synthetic food colorants in alcoholic beverages and candies by capillary electrophoresis[J].Food Sci,2014,35(14):145-150.
[12]尤妍.高效液相色谱测定雪糕中6种合成色素[J].食品研究与开发,2017,38(12):147-152.You Y.Determination of six synthetic pigments in ice cream by high performance liquid chromatography[J].Food Res Dev,2017,38(12):147-152.
[13]蒋树新,刘华良,马永建,等.在线固相萃取-高效液相色谱检测饮料中5种食用合成色素[J].分析测试学报,2016,35(12):1581-1585.Jiang SX,Liu HL,Ma YJ,et al.Determination of 5 edible synthetic pigments in drinks by online solid-phase extraction coupled with high performance liquid chromatography[J].J Instr Anal,2016,35(12):1581-1585.
[14]马莹,方灿,王其勇,等.HPLC-DAD法同时测定熏腊肉制品中的4种合成色素[J].中国食品添加剂,2014,(5):190-194.Ma Y,Fang C,Wang QY,et al.Simultaneous determination of four synthetic pigments in cured meat by HPLC-DAD[J].China Food Addit,2014,(5):190-194.
[15]鄢兵,胡俊,张云伟,等.超高效液相色谱法快速测定膨化食品中7种人工合成色素[J].中国卫生检验杂志,2014,24(2):194-197.Yan B,Hu J,Zhang YW,et al.Determination of seven synthetic pigments in puffed foods by ultra performance liquid chromatography[J].Chin JHealth Lab Technol,2014,24(2):194-197.
[16]黄志强,王飞,俞文妍,等.固相萃取-液相色谱法测定蜜饯中7种常见合成色素[J].食品安全质量检测学报,2015,6(5):1941-1947.Huang ZQ,Wang F,Yu WY,et al.Determination of 7 kinds of synthetic pigments in preserved fruits by solid-phase extraction-high performance liquid chromatography[J].J Food Saf Qual,2015,6(5):1941-1947.
[17]刘慧慧,宫向红,徐英江,等.固相萃取-高效液相色谱法同时测定海米中10种合成色素[J].食品科学,2014,35(4):170-173.Liu HH,Gong XH,Xu YJ,et al.Simultaneous determination of 10synthetic pigments in dried shrimps using solid-phase extraction-high performance liquid chromatography[J].Food Sci,2014,35(4):170-173.
[18]陈晓红,李小平,赵永纲,等.固相萃取超快速液相色谱-串联质谱同时测定熟肉制品中常用人工合成色素[J].卫生研究,2015,44(4):636-640.Chen XH,Li XP,Zhao YG,et al.An ultrafast liquid chromatography-tandem mass spectrometric method for simultaneous determination of common artificial synthetic pigments in cooked meat products[J].J Hyg Res,2015,44(4):636-640.
[19]吕东明,丁云连,詹晟,等.超高效液相色谱/四级杆-飞行时间质谱法检测22种禁用和限用合成色素[J].现代仪器与医疗,2013,19(2):52-56.Lv DM,Ding YL,Zhan S,et al.Determination of twenty two synthetic colours in beverage by ultra performance liquid chromatotraphy/quadrupole-time-of-flight mass spectrometry[J].Mod Instrum Med Treat,2013,19(2):52-56.
[20]李小平,赵永纲,陈晓红,等.固相萃取-反相高效液相色谱法同时测定葡萄酒中7种合成色素[J].中国卫生检验杂志,2013,23(12):2566-2569.Li XP,Zhao YG,Chen XH,et al.Simultaneous analysis of 7 synthetic colorants in grape wine by solid-phase extraction coupled with reversed-phase high performance liquid chromatography[J].Chin J Health Lab Technol,2013,23(12):2566-2569.
[21]GB 5009.35-2016食品中合成着色剂的测定[S].GB 5009.35-2016 Determination of synthetic colour in foods[S].
[22]李素媛,喻玺,刘恒.固相萃取-平行浓缩法测定食品中合成着色剂的研究[J].现代农业科技,2018,3:252-258.Li XY,Yu X,Liu H.Study on determination of synthetic colorants in food by solid phase extraction and parallel concentration method[J].Mod Agric Sci Technol,2018,3:252-258.
[23]高洁,宁尚勇,许志强.固相萃取-高效液相色谱法检测食品中的非食用色素[J].分析试验室,2008,27(8):33-35.Gao J,Ning SY,Xu ZQ.Solid phase extraction-liquid chromatography for simultaneous of inedible pigment in food[J].Chin J Anal Lab,2008,27(8):33-35.
[2]刘谦,李熙,吴新欣,等.高效液相色谱法同时测定复杂食品基质中8种合成色素的含量[J].理化检验-化学分册,2017,53(6):693-696.Liu Q,Li X,Wu XX,et al.Simultaneous determination of 8 kinds of synthetic cpmplex food matrix by HPLC[J].Phys Test Chem Anal B,2017,53(6):693-696.
[3]陈彦凤,肖白曼,孙彦芳,等.固相萃取-高效液相色谱法测定肉制品中合成着色剂的含量[J].中国食品卫生杂志,2013,25(5):428-430.Chen YF,Xiao BM,Sun YF,et al.Determination of synthetic colorants in meat products by SPE-HPLC[J].Chin J Food Hyg,2013,25(5):428-430.
[4]赵延胜,董英,张峰,等.食品中46种禁限用合成色素的分级提取净化体系研究[J].分析化学,2012,40(2):249-256.Zhao YS,Dong Y,Zhang F,et al.A study on system of sequential extraction and cleaning of 46 forbidden and limited synthetic pigments in food stuff[J].Chin Anal Chem,2012,40(2):249-256.
[5]毕小玲,宋娟,庄晓洪,等.固相萃取-HPLC法检测熟肉制品中合成色素[J].食品研究与开发,2017,38(5):180-183.Bi XL,Song J,Zhuang XH,et al.Determination of synthetic pigments in cooked meat by solid phase extraction and HPLC[J].Food Res Dev,2017,38(5):180-183.
[6]邹志飞,蒲民,李建军,等.各国(地区)食用色素的使用现况与比对分析[J].中国食品卫生杂志,2010,22(2):112-121.Zou ZF,Pu M,Li JJ,et al.Usage status and comparison analysis of the food colour in some countries(regions)[J].Chin J Food Hyg,2010,22(2):112-121.
[7]林芳,李涛,王一欣,等.固相萃取-超高效液相色谱法同时测定蜜饯中9种合成色素[J].食品安全质量检测学报,2016,7(2):567-574.Lin F,Li T,Wang YX,et al.Simultaneous determination of 9 kinds of synthetic pigments in preserved fruit by solid phase sxtraction-ultra high performance liquid chromatography[J].J Food Saf Qual,2016,7(2):567-574.
[8]刘艳琴,王浩,杨红梅,等.固相萃取-HPLC法同时测定糕点中8种人工合成色素[J].食品研究与开发,2010,31(2):139-142.Liu YQ,Wang H,Yang HM,et al.Determination of 8 synthetic colours in cake by solid-phase extraction couple with high performance liquid chromatography[J].Food Res Dev,2010,31(2):139-142.
[9]GB 2760-2014食品安全国家标准食品添加剂使用标准[S].GB 2760-2014 National food safety standard-Standard for uses of food additives[S].
[10]杨桂君,高文惠.毛细管电泳法测定食品中8种添加剂[J].食品科学,2010,31(8):377-380.Yang GJ,Gao WH.Determination of eight food additives in different matrices by capillary electrophoresis[J].Food Sci,2010,31(8):377-380.
[11]王丽芳,丁晓静,解娜,等.毛细管电泳法测定糖果及调制酒中10种人工合成色素[J].食品科学,2014,35(14):145-150.Wang LF,Ding XJ,Xie N,et al.Simultaneous determination of ten synthetic food colorants in alcoholic beverages and candies by capillary electrophoresis[J].Food Sci,2014,35(14):145-150.
[12]尤妍.高效液相色谱测定雪糕中6种合成色素[J].食品研究与开发,2017,38(12):147-152.You Y.Determination of six synthetic pigments in ice cream by high performance liquid chromatography[J].Food Res Dev,2017,38(12):147-152.
[13]蒋树新,刘华良,马永建,等.在线固相萃取-高效液相色谱检测饮料中5种食用合成色素[J].分析测试学报,2016,35(12):1581-1585.Jiang SX,Liu HL,Ma YJ,et al.Determination of 5 edible synthetic pigments in drinks by online solid-phase extraction coupled with high performance liquid chromatography[J].J Instr Anal,2016,35(12):1581-1585.
[14]马莹,方灿,王其勇,等.HPLC-DAD法同时测定熏腊肉制品中的4种合成色素[J].中国食品添加剂,2014,(5):190-194.Ma Y,Fang C,Wang QY,et al.Simultaneous determination of four synthetic pigments in cured meat by HPLC-DAD[J].China Food Addit,2014,(5):190-194.
[15]鄢兵,胡俊,张云伟,等.超高效液相色谱法快速测定膨化食品中7种人工合成色素[J].中国卫生检验杂志,2014,24(2):194-197.Yan B,Hu J,Zhang YW,et al.Determination of seven synthetic pigments in puffed foods by ultra performance liquid chromatography[J].Chin JHealth Lab Technol,2014,24(2):194-197.
[16]黄志强,王飞,俞文妍,等.固相萃取-液相色谱法测定蜜饯中7种常见合成色素[J].食品安全质量检测学报,2015,6(5):1941-1947.Huang ZQ,Wang F,Yu WY,et al.Determination of 7 kinds of synthetic pigments in preserved fruits by solid-phase extraction-high performance liquid chromatography[J].J Food Saf Qual,2015,6(5):1941-1947.
[17]刘慧慧,宫向红,徐英江,等.固相萃取-高效液相色谱法同时测定海米中10种合成色素[J].食品科学,2014,35(4):170-173.Liu HH,Gong XH,Xu YJ,et al.Simultaneous determination of 10synthetic pigments in dried shrimps using solid-phase extraction-high performance liquid chromatography[J].Food Sci,2014,35(4):170-173.
[18]陈晓红,李小平,赵永纲,等.固相萃取超快速液相色谱-串联质谱同时测定熟肉制品中常用人工合成色素[J].卫生研究,2015,44(4):636-640.Chen XH,Li XP,Zhao YG,et al.An ultrafast liquid chromatography-tandem mass spectrometric method for simultaneous determination of common artificial synthetic pigments in cooked meat products[J].J Hyg Res,2015,44(4):636-640.
[19]吕东明,丁云连,詹晟,等.超高效液相色谱/四级杆-飞行时间质谱法检测22种禁用和限用合成色素[J].现代仪器与医疗,2013,19(2):52-56.Lv DM,Ding YL,Zhan S,et al.Determination of twenty two synthetic colours in beverage by ultra performance liquid chromatotraphy/quadrupole-time-of-flight mass spectrometry[J].Mod Instrum Med Treat,2013,19(2):52-56.
[20]李小平,赵永纲,陈晓红,等.固相萃取-反相高效液相色谱法同时测定葡萄酒中7种合成色素[J].中国卫生检验杂志,2013,23(12):2566-2569.Li XP,Zhao YG,Chen XH,et al.Simultaneous analysis of 7 synthetic colorants in grape wine by solid-phase extraction coupled with reversed-phase high performance liquid chromatography[J].Chin J Health Lab Technol,2013,23(12):2566-2569.
[21]GB 5009.35-2016食品中合成着色剂的测定[S].GB 5009.35-2016 Determination of synthetic colour in foods[S].
[22]李素媛,喻玺,刘恒.固相萃取-平行浓缩法测定食品中合成着色剂的研究[J].现代农业科技,2018,3:252-258.Li XY,Yu X,Liu H.Study on determination of synthetic colorants in food by solid phase extraction and parallel concentration method[J].Mod Agric Sci Technol,2018,3:252-258.
[23]高洁,宁尚勇,许志强.固相萃取-高效液相色谱法检测食品中的非食用色素[J].分析试验室,2008,27(8):33-35.Gao J,Ning SY,Xu ZQ.Solid phase extraction-liquid chromatography for simultaneous of inedible pigment in food[J].Chin J Anal Lab,2008,27(8):33-35.