高效液相色谱法同时测定果冻、口香糖和明胶囊壳中11种合成着色剂及其8种铝色淀
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摘要
目的建立高效液相色谱法测定果冻、口香糖和明胶囊壳中11种合成着色剂及8种铝色淀的含量。方法样品经提取溶剂(乙醇:2%氨水:水=7:2:1,V:V:V)2次超声提取,离心后的上清液经固相萃取柱净化,用Agilent SB-C18 (4.6 mm×250 mm, 5μm)柱分离, 0.02 mol/L乙酸铵水溶液-甲醇作为流动相梯度洗脱,二极管阵列检测器检测,外标法定量。结果 11种合成着色剂在0.1～10 mg/L范围内与峰面积呈良好线性关系,相关系数均达到0.9999,方法精密度良好,相对标准偏差(relative standard deviation, RSD)为1.4%～3.9%(n=6)。11种着色剂加标回收率为80.1%～110%, RSD为0.15%～5.5%(n=3), 8种铝色淀加标回收率为80.8%～105.6%, RSD为0.4%～5.4%(n=3)。检出限为0.1～0.4 mg/kg,定量限为0.2～1.1 mg/kg。结论该方法简便灵敏,准确可靠,适用于果冻、口香糖和明胶胶囊壳中合成着色剂及铝色淀的测定。
Objective To establish a method for the determination of 11 kinds of synthetic colorants and 8 kinds of aluminum lakes in the jelly,chewing gum and capsule shell by high performance liquid chromatography.Methods The sample was extracted twice by ultrasonic extraction solvent(ethanol: 2% ammonia: water=7:2:1,V:V:V),the supernatant after centrifugation was purified by solid phase extraction column,and separated by Agilent SB-C18 column(4.6 mm×250 mm,5 μm) at the flow rate of 0.02 mol/L by gradient elution using with the 0.02 mol/L ammonium acetate aqueous solution-methanol,then detected by diode array detector,and quantitated by external standard method.Results There were linear relationships between the peak areas of 11 compounds in the range of 0.1-10 mg/L and the correlation coefficients were all greater than 0.9999.Precisions of method were good with the relative standard deviations(RSDs) of 1.4%-3.9%(n=6).Recoveries of 11 kinds of colorants were 80.1%-110%,and the RSDs were 0.15%-5.5%(n=3).The recoveries of 8 kinds of aluminum lakes were 80.8%-105.6%,and the RSDs were 0.4%-5.4%(n=3).The limits of detection and limits of quantitative ranged within 0.1-0.4 mg/kg and 0.2-1.1 mg/kg,respectively.Conclusion The method is simple,rapid and sensitive,which is suitable for the determination of 11 kinds of synthetic pigments and 8 kinds of aluminum lakes in jelly,chewing gum and capsule shell.
Objective To establish a method for the determination of 11 kinds of synthetic colorants and 8 kinds of aluminum lakes in the jelly,chewing gum and capsule shell by high performance liquid chromatography.Methods The sample was extracted twice by ultrasonic extraction solvent(ethanol: 2% ammonia: water=7:2:1,V:V:V),the supernatant after centrifugation was purified by solid phase extraction column,and separated by Agilent SB-C18 column(4.6 mm×250 mm,5 μm) at the flow rate of 0.02 mol/L by gradient elution using with the 0.02 mol/L ammonium acetate aqueous solution-methanol,then detected by diode array detector,and quantitated by external standard method.Results There were linear relationships between the peak areas of 11 compounds in the range of 0.1-10 mg/L and the correlation coefficients were all greater than 0.9999.Precisions of method were good with the relative standard deviations(RSDs) of 1.4%-3.9%(n=6).Recoveries of 11 kinds of colorants were 80.1%-110%,and the RSDs were 0.15%-5.5%(n=3).The recoveries of 8 kinds of aluminum lakes were 80.8%-105.6%,and the RSDs were 0.4%-5.4%(n=3).The limits of detection and limits of quantitative ranged within 0.1-0.4 mg/kg and 0.2-1.1 mg/kg,respectively.Conclusion The method is simple,rapid and sensitive,which is suitable for the determination of 11 kinds of synthetic pigments and 8 kinds of aluminum lakes in jelly,chewing gum and capsule shell.
引文
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[5]王硕,张向明,毛红霞,等.高效液相色谱法同时测定糖果中6种合成着色剂及其铝色淀[J].现代预防医学,2016,43(22):4174-4178.Wang S,Zhang XM,Mao HX,et al.Simultaneous determination of 6synthetic colorants and their aluminum lakes in candies by HPLC[J].Mod Prev Med,2016,43(22):4174-4178.
[6]肖亮,于忠飞,薛芳,等.聚酰胺小柱净化-反相液相色谱同时测定海米中4种合成着色剂[J].中国食品添加剂,2014,(6):167-171.Xiao L,Yu ZF,Xue F,et al.Simultaneous determination of four synthetic colourants in dried shrimps by polyamide cartridge and HPLC[J].China Food Addit,2014,(6):167-171.
[7]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-Standards for the use of food additives[S].
[8]GB/T 5009.35-2016食品中合成着色剂的测定[S].GB/T 5009.35-2016 Determination of synthetic colorants in foods[S].
[9]赵鹏,黄亚琴,徐奋奋,等.固相萃取-高效液相色谱-可变波长检测法测定鲜榨果汁中7种水溶性合成着色剂[J].中国卫生检验杂志,2015,25(8):1159.Zhao P,Huang YQ,Xu FF,et al.Determination of 7 kinds of water-soluble synthetic colorants in fresh juice by SPE-HPLC and variable wavelength detection[J].Chin J Health Lab Technol,2015,25(8):1159.
[10]张勋,邢燕燕,赵韫慧,等.基于液相色谱-串联质谱法检测多种食品中的16种合成着色剂[J].化学试剂,2017,39(4):385-390.Zhang X,Xing YY,Zhao YH,et al.Determination of 16 synthetic colorants in various foods by LC-MS/MS method[J].Chem Reag,2017,39(4):385-390
[11]李晓芹,徐振东.固相萃取-高效液相色谱法在食品中合成着色剂检测中的应用[J].食品工业,2014,35(6):56-58.Li XQ,Xu ZD.Determination of synthetic colorants in food by SPE-HPLC[J].Food Ind,2014,35(6):56-58
[12]李娜,李淑娟,宋娟,等.快速液相色谱法测定食品中11种合成着色剂[J].食品工业科技,2009,30(1):313-315.Li N,Li SJ,Song J,et al Determination of eleven synthetic colorants in food by rapid resolution liquid chromatography[J].Sci Technol Food Ind,2009,30(1):313-315.
[13]马桂娟,汤丽华,朱捷,等.固相萃取-高效液相色谱法快速测定食品中7种合成着色剂[J].食品安全导刊,2017,(36):53-54.Ma GJ,Tang LH,Zhu J,et al.Rapid determination of 7 synthetic colouring agents in food by solid phase extraction-high performance liquid chromatography[J].China Food Saf Mag,2017,(36):53-54.
[14]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):180-183Bi 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.
[15]杨晓倩,刘素华,曹小丽.固相萃取-超高效液相色谱法同时测定肉制品中5种合成着色剂[J].食品与药品,2015,17(4):259-262.Yang XQ,Liu SH,Cao XL.Simultaneous analysis of five kinds of synthetic colorants in meat products by SPE-UPLC[J].Food Drug,2015,17(4):259-262.
[2]杨昊,王骏,周莉莉,等.虾籽中十种合成色素及其色淀的高效液相色谱测定方法[J].山东农业科学,2014,46(1):110-113.Yang H,Wang J,Zhou LL,et al.Determination of ten synthetic colorants and their aluminum lakes in shrimp eggs by high performance liquid chromatography[J].Shandong Agric Sci,2014,46(1):110-113.
[3]薛虎寅,尹永梅,张太昌,等.偶氮类合成色素检测技术的研究进展[J].生物技术进展,2012,2(3):171-176.Xue HY,Yin YM,Zhang TC,et al.Research on analysis of azo dyes in food products[J].Curr Biotechnol,2012,2(3):171-176.
[4]Yang Y,Yin J,Shao B.Simultaneous determination of five Aluminum lake dyes in chewing gum by HPLC with photodiode array detection[J].Food Addit Contam Part A-Chem Anal Control Expos Risk Assess,2011,28(9):1159-1167.
[5]王硕,张向明,毛红霞,等.高效液相色谱法同时测定糖果中6种合成着色剂及其铝色淀[J].现代预防医学,2016,43(22):4174-4178.Wang S,Zhang XM,Mao HX,et al.Simultaneous determination of 6synthetic colorants and their aluminum lakes in candies by HPLC[J].Mod Prev Med,2016,43(22):4174-4178.
[6]肖亮,于忠飞,薛芳,等.聚酰胺小柱净化-反相液相色谱同时测定海米中4种合成着色剂[J].中国食品添加剂,2014,(6):167-171.Xiao L,Yu ZF,Xue F,et al.Simultaneous determination of four synthetic colourants in dried shrimps by polyamide cartridge and HPLC[J].China Food Addit,2014,(6):167-171.
[7]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-Standards for the use of food additives[S].
[8]GB/T 5009.35-2016食品中合成着色剂的测定[S].GB/T 5009.35-2016 Determination of synthetic colorants in foods[S].
[9]赵鹏,黄亚琴,徐奋奋,等.固相萃取-高效液相色谱-可变波长检测法测定鲜榨果汁中7种水溶性合成着色剂[J].中国卫生检验杂志,2015,25(8):1159.Zhao P,Huang YQ,Xu FF,et al.Determination of 7 kinds of water-soluble synthetic colorants in fresh juice by SPE-HPLC and variable wavelength detection[J].Chin J Health Lab Technol,2015,25(8):1159.
[10]张勋,邢燕燕,赵韫慧,等.基于液相色谱-串联质谱法检测多种食品中的16种合成着色剂[J].化学试剂,2017,39(4):385-390.Zhang X,Xing YY,Zhao YH,et al.Determination of 16 synthetic colorants in various foods by LC-MS/MS method[J].Chem Reag,2017,39(4):385-390
[11]李晓芹,徐振东.固相萃取-高效液相色谱法在食品中合成着色剂检测中的应用[J].食品工业,2014,35(6):56-58.Li XQ,Xu ZD.Determination of synthetic colorants in food by SPE-HPLC[J].Food Ind,2014,35(6):56-58
[12]李娜,李淑娟,宋娟,等.快速液相色谱法测定食品中11种合成着色剂[J].食品工业科技,2009,30(1):313-315.Li N,Li SJ,Song J,et al Determination of eleven synthetic colorants in food by rapid resolution liquid chromatography[J].Sci Technol Food Ind,2009,30(1):313-315.
[13]马桂娟,汤丽华,朱捷,等.固相萃取-高效液相色谱法快速测定食品中7种合成着色剂[J].食品安全导刊,2017,(36):53-54.Ma GJ,Tang LH,Zhu J,et al.Rapid determination of 7 synthetic colouring agents in food by solid phase extraction-high performance liquid chromatography[J].China Food Saf Mag,2017,(36):53-54.
[14]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):180-183Bi 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.
[15]杨晓倩,刘素华,曹小丽.固相萃取-超高效液相色谱法同时测定肉制品中5种合成着色剂[J].食品与药品,2015,17(4):259-262.Yang XQ,Liu SH,Cao XL.Simultaneous analysis of five kinds of synthetic colorants in meat products by SPE-UPLC[J].Food Drug,2015,17(4):259-262.