高效液相色谱法测定饮料中12种水溶性合成着色剂
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摘要
目的建立高效液相色谱法同时测定饮料中柠檬黄、喹啉黄、苋菜红、胭脂红、日落黄、诱惑红、酸性红、赤藓红、靛蓝、酸性绿S、亮蓝、专利蓝V 12种水溶性合成着色剂的方法。方法饮料样品经离心、过滤后直接进样,以甲醇-乙酸铵(0.02 mol/L)为流动相进行梯度洗脱,采用二极管阵列检测器多波长分析,外标法定量。结果 12种合成着色剂在0.5～100mg/L范围内线性关系良好,相关系数均大于0.999;检出限为0.05～0.3 mg/kg;平均回收率为91.0%～101.3%,相对标准偏差值为0.2%～2.3%。结论该方法简便、快速、准确,前处理简单,适合于基质成分较为简单的液体样品中多种着色剂的同时测定。
Objective To establish a method for determination of 12 kinds of water-soluble synthetic colorants(tartrazine,quinoline yellow,amaranth,carmine,sunset yellow,allura red,carmosine,erythrosine,indigotin,green S,brilliant blue,patent blue V) in drinks by high performance liquid chromatography(HPLC).Methods The drink samples were centrifuged and filtered,then the sample solutions were injected into HPLC with diode array detection and detected at different wavelength.The mobile phase was methanol-0.02 mol/L ammonium acetate with gradient elution.The external standard method was adopted for quantification of the analytes.Results The linear range of 12 water-soluble synthetic colorants were 0.5-100 mg/L with the correlation coefficients were higher than 0.999.The limits of detection were from 0.05 to 0.3 mg/kg.The average recoveries were from 91.0% to 101.3%,and the relative standard deviations(RSDs) were from 0.2% to 2.3%.Conclusion This method is simple,quick and accurate,which can be applied to detect synthetic colorants simultaneously in uncomplicated liquid foods.
Objective To establish a method for determination of 12 kinds of water-soluble synthetic colorants(tartrazine,quinoline yellow,amaranth,carmine,sunset yellow,allura red,carmosine,erythrosine,indigotin,green S,brilliant blue,patent blue V) in drinks by high performance liquid chromatography(HPLC).Methods The drink samples were centrifuged and filtered,then the sample solutions were injected into HPLC with diode array detection and detected at different wavelength.The mobile phase was methanol-0.02 mol/L ammonium acetate with gradient elution.The external standard method was adopted for quantification of the analytes.Results The linear range of 12 water-soluble synthetic colorants were 0.5-100 mg/L with the correlation coefficients were higher than 0.999.The limits of detection were from 0.05 to 0.3 mg/kg.The average recoveries were from 91.0% to 101.3%,and the relative standard deviations(RSDs) were from 0.2% to 2.3%.Conclusion This method is simple,quick and accurate,which can be applied to detect synthetic colorants simultaneously in uncomplicated liquid foods.
引文
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[2]朱海英,黄万琪.食品安全法背景下合成色素的问题及对策[J].现代医药卫生,2011,27(8):1259-1261.Zhu HY,Huang WQ.On synthetic pigment problems and countermeasures in background of food safety law[J].J Mod Med Health,2011,27(8):1259-1261.
[3]阎炳宗.食用着色剂发展趋势[J].食品科技,2004,(2):47-51.Yan BZ.Trends in Chinese food color industry[J].Food Sci Technol,2004,(2):47-51.
[4]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].
[5]阮丽萍,吉文亮,刘华良,等.高效液相色谱法同时测定食品中10种合成着色剂[J].中国食品卫生杂志,2011,23(2):151-154.Ruan LP,Ji WL,Liu HL,et al.Simultaneous determination of 10synthetic colorants in foods with high performance liquid chromatography[J].Chin J Food Hyg,2011,23(2):151-154.
[6]杨勇,罗奕,吴琳琳,等.HPLC-DAD法测定馒头中喹啉黄、食用绿S和亮绿3种色素含量的研究[J].粮油食品科技,2015,23(6):71-75.Yang Y,Luo Y,Wu LL,et al.Study on determination of 3 kinds of pigments content of yellow,green S and bright green in steamed bread by HPLC-DAD method[J].Sci Technol Cere Oil Foods,2015,23(6):71-75.
[7]刘泰然,赵海燕,罗仁才.超高效液相色谱法同时测定饮料中的17种食品添加剂[J].中国食品卫生杂志,2013,25(1):44-48.Liu TR,Zhao HY,Luo RC.Simultaneous determination of 17 food additives in drinks by ultra high performance liquid chromatography[J].Chin J Food Hyg,2013,25(1):44-48.
[8]肖海龙,屠海云,王红青,等.反相高效液相色谱法快速测定食品中18种水溶性合成着色剂[J].中国卫生检验杂志,2011,21(2):264-266.Xiao HL,Tu HY,Wang HQ,et al.Rapid method for simultaneous determination of 18 water-soluble synthetic pigments in food by RP-HPLC[J].Chin J Health Lab Technol,2011,21(2):264-266.
[9]谭慧,王胜,朱其名.高效液相色谱法同时测定熟肉制品中的10种合成色素[J].中国卫生检验杂志,2014,24(16):2334-2336.Tan H,Wang S,Zhu QM.Simultaneous determination of 10 synthetic pigments in cooked meat products by high performance liquid chromatography[J].Chin J Health Lab Technol,2014,24(16):2334-2336.
[10]李帮锐,冯家力,潘振球,等.高效液相色谱-质谱/质谱联用法测定饮料中的人工合成色素[J].中国卫生检验杂志,2007,17(4):579-580,585.Li BR,Feng JL,Pan ZQ,et al.Determination of synthetical pigments in drinks by high performance liquid chromatography-mass spectrometry/mass spectrometry[J].Chin J Health Lab Technol,2007,17(4):579-580,585.
[11]伊雄海,邓晓军,杨惠琴,等.液相色谱-串联质谱法检测食品中的多种易滥用着色剂[J].色谱,2011,29(11):1062-1069.Yin XH,Deng XJ,Yang HQ,et al.Determination of commonly abused dyes in food by liquid chromatography-tandem mass spectrometry[J].Chin J Chromatogr,2011,29(11):1062-1069.
[12]Morlock G,Oellig C.食品中25种水溶性色素的HPTLC同时含量测定[C].第四届国际食品安全高峰论坛论文集,2011,89-92.Morlock G,Oellig C.Simultaneous determination of 25 water-soluble pigments in food by HPTLC[C].Essay Collect Fourth Int Food Safe Forum,2011,89-92.
[13]李德金,赵明哲,栾广杰.示波极谱法测定食品中人工合成色素的探讨[J].食品研究与开发,2004,25(6):107-108.Li DJ,Zhao MZ,Luan GJ.Determination of synthetic pigments in food by oscillopolarography[J].Food Res Dev,2004,25(6):107-108.
[14]龙巍然,王兴益,史振雨,等.胶束电动毛细管色谱同时测定食品中13种人工合成色素[J].分析测试学报,2012,31(9):1100-1104.Long WR,Wang XY,Shi ZY,et al.Determination of thirteen artificially synthesized pigments in food by micellar electrokinetic capillary chromatography[J].J Instrum Anal,2012,31(9):1100-1104.
[15]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.
[16]龙巍然,岑怡红,王兴益,等.毛细管区带电泳法同时测定饮料中16种食品添加剂[J].色谱,2012,30(7):747-751.Long WR,Cen YH,Wang XY,et al.Determination of sixteen food additives in beverage by capillary zone electrophoresis[J].Chin JChromatogr,2012,30(7):747-751.
[17]郑新华,王乐,韩焕美,等.液相色谱串联质谱法检测食品中4种人工合成着色剂[J].食品安全质量检测学报,2016,7(4):1412-1418.Zheng XH,Wang L,Han HM,et al.Determination of 4 kinds of synthetic colorants in food by liquid chromatography-tandem mass spectrometry[J].J Food Saf Qual,2016,7(4):1412-1418.
[18]林慧,徐春祥,刘成志,等.液相色谱-串联四极杆飞行时间质谱快速筛查食品中违禁着色剂[J].食品安全质量检测学报,2017,8(4):1389-1396.Lin H,Xu CX,Liu CZ,et al.Rapid screening of banned pigments in food by liquid chromatography-tandem quadrupole time of flight mass spectrometry[J].J Food Saf Qual,2017,8(4):1389-1396.
[19]Séverine G,Vincent H,Hasna T,et al.Determination of caramel colorants’by-products in liquid foods by ultra-high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)[J].Food Addit Contam A,2014,31(10):1652-1660.
[20]Andrade FI,Florindo GMI,Pinto VIG,et al.Determination of synthetic food dyes in commercial soft drinks by TLC and ion-pair HPLC[J].Food Chem,2014,157:193-198.
[21]GB 5009.35-2016食品安全国家标准食品中合成着色剂的测定[S].GB 5009.35-2016 National food safety standard-Determination of synthetic colorant in foods[S].
[22]GB 5009.141-2016食品安全国家标准食品中诱惑红的测定[S].GB 5009.141-2016 National food safety standard-Determination of allura red in foods[S].
[23]SN/T 1743-2006食品中的诱惑红、酸性红、亮蓝、日落黄的含量检测高效液相色谱法[S].SN/T 1743-2006 Determination of allura red AC,carmosine,brilliant blue FCF,sunset yellow FCF in food-High performance liquid chromatographic method[S].
[2]朱海英,黄万琪.食品安全法背景下合成色素的问题及对策[J].现代医药卫生,2011,27(8):1259-1261.Zhu HY,Huang WQ.On synthetic pigment problems and countermeasures in background of food safety law[J].J Mod Med Health,2011,27(8):1259-1261.
[3]阎炳宗.食用着色剂发展趋势[J].食品科技,2004,(2):47-51.Yan BZ.Trends in Chinese food color industry[J].Food Sci Technol,2004,(2):47-51.
[4]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].
[5]阮丽萍,吉文亮,刘华良,等.高效液相色谱法同时测定食品中10种合成着色剂[J].中国食品卫生杂志,2011,23(2):151-154.Ruan LP,Ji WL,Liu HL,et al.Simultaneous determination of 10synthetic colorants in foods with high performance liquid chromatography[J].Chin J Food Hyg,2011,23(2):151-154.
[6]杨勇,罗奕,吴琳琳,等.HPLC-DAD法测定馒头中喹啉黄、食用绿S和亮绿3种色素含量的研究[J].粮油食品科技,2015,23(6):71-75.Yang Y,Luo Y,Wu LL,et al.Study on determination of 3 kinds of pigments content of yellow,green S and bright green in steamed bread by HPLC-DAD method[J].Sci Technol Cere Oil Foods,2015,23(6):71-75.
[7]刘泰然,赵海燕,罗仁才.超高效液相色谱法同时测定饮料中的17种食品添加剂[J].中国食品卫生杂志,2013,25(1):44-48.Liu TR,Zhao HY,Luo RC.Simultaneous determination of 17 food additives in drinks by ultra high performance liquid chromatography[J].Chin J Food Hyg,2013,25(1):44-48.
[8]肖海龙,屠海云,王红青,等.反相高效液相色谱法快速测定食品中18种水溶性合成着色剂[J].中国卫生检验杂志,2011,21(2):264-266.Xiao HL,Tu HY,Wang HQ,et al.Rapid method for simultaneous determination of 18 water-soluble synthetic pigments in food by RP-HPLC[J].Chin J Health Lab Technol,2011,21(2):264-266.
[9]谭慧,王胜,朱其名.高效液相色谱法同时测定熟肉制品中的10种合成色素[J].中国卫生检验杂志,2014,24(16):2334-2336.Tan H,Wang S,Zhu QM.Simultaneous determination of 10 synthetic pigments in cooked meat products by high performance liquid chromatography[J].Chin J Health Lab Technol,2014,24(16):2334-2336.
[10]李帮锐,冯家力,潘振球,等.高效液相色谱-质谱/质谱联用法测定饮料中的人工合成色素[J].中国卫生检验杂志,2007,17(4):579-580,585.Li BR,Feng JL,Pan ZQ,et al.Determination of synthetical pigments in drinks by high performance liquid chromatography-mass spectrometry/mass spectrometry[J].Chin J Health Lab Technol,2007,17(4):579-580,585.
[11]伊雄海,邓晓军,杨惠琴,等.液相色谱-串联质谱法检测食品中的多种易滥用着色剂[J].色谱,2011,29(11):1062-1069.Yin XH,Deng XJ,Yang HQ,et al.Determination of commonly abused dyes in food by liquid chromatography-tandem mass spectrometry[J].Chin J Chromatogr,2011,29(11):1062-1069.
[12]Morlock G,Oellig C.食品中25种水溶性色素的HPTLC同时含量测定[C].第四届国际食品安全高峰论坛论文集,2011,89-92.Morlock G,Oellig C.Simultaneous determination of 25 water-soluble pigments in food by HPTLC[C].Essay Collect Fourth Int Food Safe Forum,2011,89-92.
[13]李德金,赵明哲,栾广杰.示波极谱法测定食品中人工合成色素的探讨[J].食品研究与开发,2004,25(6):107-108.Li DJ,Zhao MZ,Luan GJ.Determination of synthetic pigments in food by oscillopolarography[J].Food Res Dev,2004,25(6):107-108.
[14]龙巍然,王兴益,史振雨,等.胶束电动毛细管色谱同时测定食品中13种人工合成色素[J].分析测试学报,2012,31(9):1100-1104.Long WR,Wang XY,Shi ZY,et al.Determination of thirteen artificially synthesized pigments in food by micellar electrokinetic capillary chromatography[J].J Instrum Anal,2012,31(9):1100-1104.
[15]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.
[16]龙巍然,岑怡红,王兴益,等.毛细管区带电泳法同时测定饮料中16种食品添加剂[J].色谱,2012,30(7):747-751.Long WR,Cen YH,Wang XY,et al.Determination of sixteen food additives in beverage by capillary zone electrophoresis[J].Chin JChromatogr,2012,30(7):747-751.
[17]郑新华,王乐,韩焕美,等.液相色谱串联质谱法检测食品中4种人工合成着色剂[J].食品安全质量检测学报,2016,7(4):1412-1418.Zheng XH,Wang L,Han HM,et al.Determination of 4 kinds of synthetic colorants in food by liquid chromatography-tandem mass spectrometry[J].J Food Saf Qual,2016,7(4):1412-1418.
[18]林慧,徐春祥,刘成志,等.液相色谱-串联四极杆飞行时间质谱快速筛查食品中违禁着色剂[J].食品安全质量检测学报,2017,8(4):1389-1396.Lin H,Xu CX,Liu CZ,et al.Rapid screening of banned pigments in food by liquid chromatography-tandem quadrupole time of flight mass spectrometry[J].J Food Saf Qual,2017,8(4):1389-1396.
[19]Séverine G,Vincent H,Hasna T,et al.Determination of caramel colorants’by-products in liquid foods by ultra-high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)[J].Food Addit Contam A,2014,31(10):1652-1660.
[20]Andrade FI,Florindo GMI,Pinto VIG,et al.Determination of synthetic food dyes in commercial soft drinks by TLC and ion-pair HPLC[J].Food Chem,2014,157:193-198.
[21]GB 5009.35-2016食品安全国家标准食品中合成着色剂的测定[S].GB 5009.35-2016 National food safety standard-Determination of synthetic colorant in foods[S].
[22]GB 5009.141-2016食品安全国家标准食品中诱惑红的测定[S].GB 5009.141-2016 National food safety standard-Determination of allura red in foods[S].
[23]SN/T 1743-2006食品中的诱惑红、酸性红、亮蓝、日落黄的含量检测高效液相色谱法[S].SN/T 1743-2006 Determination of allura red AC,carmosine,brilliant blue FCF,sunset yellow FCF in food-High performance liquid chromatographic method[S].