柱前衍生法测定功能性饮料与口服液中的牛磺酸
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摘要
采用丹磺酰氯柱前衍生法检测功能性饮料和口服液中的牛磺酸的含量,使用高效液相色谱(high performance liquid chromatography,HPLC)分析衍生产物,其中色谱配有可变波长紫外检测器,检测器波长设为254 nm。选用C18色谱柱进行产物分离,流动相选用乙酸钠水溶液-乙腈(30∶70,体积比)等度洗脱,柱温设为25℃,样品进样量为5μL。检测结果表明牛磺酸浓度为5μg/mL～50μg/L时,牛磺酸衍生物峰面积对浓度呈现良好的线性关系,相关系数为0.999。采用单因素和正交试验相结合的方法确定了最佳反应条件。结果表明衍生温度35℃,衍生时间35 min,衍生剂用量300μL,衍生溶液pH 9.5时,衍生物峰面积达到最大。在此试验条件下6组重复性试验衍生物峰面积相对标准偏差(relative standard deviation,RSD)为1.4%,重复性较好。对功能性饮料和口服液中牛磺酸进行检测,测量值与标识值误差在-10.0%～+10.0%,样品加标回收率为90.0%～108.0%,样品平行测试的偏差小于3.0%,此种方法反应条件温和,操作简单。
Taurine in energy drinks and oral liquid was determined by pre-column derivatization with dansyl chloride. The derivatives were detected by high performance liquid chromatography(HPLC). HPLC with variable wavelength detector was selected,and the wavelength was set at 254 nm. C18 column was used to separate the derivatives,and the sodium acetate solution and acetonitrile(30 ∶ 70,volume ratio)was used as mobile phase for isometric elution. The column temperature was set at 25 ℃ and the sample injection volume was 5 μL. When the concentration of taurine was 5 μg/mL-50 μg/L,the peak area of taurine derivatives had a good linear relationship with the concentration and the correlation coefficient was 0.999. The combination of single factor and orthogonal experiment was used to optimize the derivatization experiment conditions. The results of the test had shown that the peak area of the derivative reached the maximum when derivatization temperature was 35 ℃,derivatization time was 35 min,the volume of derivatization reagent was 300 μL and the pH value of the derivative solution was 9.5. Under the experimental conditions,the relative standard deviation(RSD)of the peak area of the six groups was 1.4 % and the repeatability was good. The content of taurine in energy drinks and oral liquid was detected,and the recovery rate was 90.0 %-108.0 %. The deviation between the measured value and the identified value was-10.0 %-+10.0 %,the deviation of the parallel test is less than 3.0 %. Therefore,this method had the advantages of easy preparation and mild reaction conditions.
Taurine in energy drinks and oral liquid was determined by pre-column derivatization with dansyl chloride. The derivatives were detected by high performance liquid chromatography(HPLC). HPLC with variable wavelength detector was selected,and the wavelength was set at 254 nm. C18 column was used to separate the derivatives,and the sodium acetate solution and acetonitrile(30 ∶ 70,volume ratio)was used as mobile phase for isometric elution. The column temperature was set at 25 ℃ and the sample injection volume was 5 μL. When the concentration of taurine was 5 μg/mL-50 μg/L,the peak area of taurine derivatives had a good linear relationship with the concentration and the correlation coefficient was 0.999. The combination of single factor and orthogonal experiment was used to optimize the derivatization experiment conditions. The results of the test had shown that the peak area of the derivative reached the maximum when derivatization temperature was 35 ℃,derivatization time was 35 min,the volume of derivatization reagent was 300 μL and the pH value of the derivative solution was 9.5. Under the experimental conditions,the relative standard deviation(RSD)of the peak area of the six groups was 1.4 % and the repeatability was good. The content of taurine in energy drinks and oral liquid was detected,and the recovery rate was 90.0 %-108.0 %. The deviation between the measured value and the identified value was-10.0 %-+10.0 %,the deviation of the parallel test is less than 3.0 %. Therefore,this method had the advantages of easy preparation and mild reaction conditions.
引文
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[13]康明芹,陈明岩,王岸英,等.超高效液相色谱-蒸发光散射法测定功能性饮料中牛磺酸[J].分析试验室,2016,35(9):1030-1032
[14]娄婷婷,赵婷,温华蔚,等.婴儿食品中牛磺酸含量测定及其不确定度分析[J].食品研究与开发,2016,37(24):120-124
[15]王晓莺,孙成均,杨元,等.FMOC柱前衍生-高效液相色谱法测定饮料中的牛磺酸[J].现代预防医学,2006,33(3):371-373
[16]张博,刘思洁,石矛,等.邻苯二甲醛-柱后衍生-高效液相色谱荧光法测定功能型饮料中的牛磺酸[J].中国卫生检验杂志,2016,26(3):345-346
[17]魏永涛,林娣,曹广生.柱后衍生HPLC法测定功能饮料中的牛磺酸[J].化学分析计量,2017,26(6):41-44
[18]黄岛平,陈秋虹,劳燕文.柱前衍生高效液相色谱法测定红牛维生素功能饮料中牛磺酸含量[J].广西科学院学报,2006,22(z1):419-421
[19]郭升平.柱前衍生化反相HPLC法测定几种营养口服液中的牛磺酸[J].福建分析测试,1996,5(4):579-580
[20]冯盛斌,胡海娥.PITC柱前衍生反相高效液相色谱法测定维生素功能饮料中L-赖氨酸和牛磺酸的含量[J].饮料工业,2014,17(4):38-40
[21]柯加法,华永有,黄宏南.柱前衍生-HPLC法测定口服液类保健食品中的牛磺酸[J].海峡预防医学杂志,2009,15(3):13-15
[22]方灿.柱前衍生-高效液相色谱法测定七维牛磺酸口服溶液中牛磺酸的含量[J].药物分析杂志,2007,27(7):1102-1104
[23]顾丽娟,严相平.柱前衍生化法测定五维牛磺酸口服液中牛磺酸的含量[J].江苏医药,2010,36(8):979-980
[24]张晓凤,邹晓莉,曾红燕.2,4-二硝基氯苯衍生高效液相色谱法测定饮品中牛磺酸含量[J].分析试验室,2012,31(6):46-49
[25]朱慧,赵志红,施文蓉.应用单磺酰氯柱前衍生法测定食品中的牛磺酸[J].食品科学,2000,21(12):116-118
[26]WOOLLARD D C,INDYK H E.Taurine analysis in milk and infant formulae by liquid chromatography:collaborative study[J].Journal of Aoac International,1997,80(4):860-865
[27]BIONDI P A,MANCA F,NEGRI A.HPLC determination of plasma taurine[J].Chromatographia,1987,24(1):360-362
[28]中华人民共和国国家卫生和计划生育委员会.食品安全国家标准食品中牛磺酸的测定:GB5009.169-2016[S].北京:中国标准出版社,2017
[2]杨祖英,张平伟.高效液相色谱法测定食品中的牛磺酸[J].卫生研究,1998,27(3):192-194
[3]高亚,郭俊霞,张艳贞,等.牛磺酸降血糖作用研究进展[J].中国食品学报,2016,16(1):202-210
[4]徐莉,陈文慧,符灵梅,等.近海养殖牡蛎中牛磺酸含量检测方法研究[J].食品研究与开发,2015,36(18):151-153
[5]高加龙,章超桦,邱伟佳,等.南海不同产地近江牡蛎中牛磺酸含量检测[J].食品科学,2013,34(10):164-168
[6]徐成,卢虹玉,章超桦,等.超高压法提取牡蛎中牛磺酸的工艺研究[J].食品工业科技,2016,37(19):192-196
[7]王芬,张婷,顾振新,等.高效液相色谱法测定紫菜中牛磺酸含量[J].食品科学,2012,33(18):162-164
[8]李则均.人乳与牛乳中牛磺酸含量测定比较[J].中国奶牛,2017,325(5):32-35
[9]李珊,刘玉兰.荧光法测定食物中牛磺酸[J].理化检验(化学分册),2001,37(2):80-81
[10]劳燕文,杨益林.母乳泉口服液中牛磺酸的测定[J].现代仪器与医疗,2006,12(1):65-66
[11]陈季凤.解决儿童营养液中牛磺酸的薄层色谱鉴定法[J].现代中药研究与实践,1994,8(3):28
[12]李秀花,邱服斌,肖荣,等.紫外分光光度法测定动物脑组织中牛磺酸含量[J].山西医药杂志,2001,30(3):209-210
[13]康明芹,陈明岩,王岸英,等.超高效液相色谱-蒸发光散射法测定功能性饮料中牛磺酸[J].分析试验室,2016,35(9):1030-1032
[14]娄婷婷,赵婷,温华蔚,等.婴儿食品中牛磺酸含量测定及其不确定度分析[J].食品研究与开发,2016,37(24):120-124
[15]王晓莺,孙成均,杨元,等.FMOC柱前衍生-高效液相色谱法测定饮料中的牛磺酸[J].现代预防医学,2006,33(3):371-373
[16]张博,刘思洁,石矛,等.邻苯二甲醛-柱后衍生-高效液相色谱荧光法测定功能型饮料中的牛磺酸[J].中国卫生检验杂志,2016,26(3):345-346
[17]魏永涛,林娣,曹广生.柱后衍生HPLC法测定功能饮料中的牛磺酸[J].化学分析计量,2017,26(6):41-44
[18]黄岛平,陈秋虹,劳燕文.柱前衍生高效液相色谱法测定红牛维生素功能饮料中牛磺酸含量[J].广西科学院学报,2006,22(z1):419-421
[19]郭升平.柱前衍生化反相HPLC法测定几种营养口服液中的牛磺酸[J].福建分析测试,1996,5(4):579-580
[20]冯盛斌,胡海娥.PITC柱前衍生反相高效液相色谱法测定维生素功能饮料中L-赖氨酸和牛磺酸的含量[J].饮料工业,2014,17(4):38-40
[21]柯加法,华永有,黄宏南.柱前衍生-HPLC法测定口服液类保健食品中的牛磺酸[J].海峡预防医学杂志,2009,15(3):13-15
[22]方灿.柱前衍生-高效液相色谱法测定七维牛磺酸口服溶液中牛磺酸的含量[J].药物分析杂志,2007,27(7):1102-1104
[23]顾丽娟,严相平.柱前衍生化法测定五维牛磺酸口服液中牛磺酸的含量[J].江苏医药,2010,36(8):979-980
[24]张晓凤,邹晓莉,曾红燕.2,4-二硝基氯苯衍生高效液相色谱法测定饮品中牛磺酸含量[J].分析试验室,2012,31(6):46-49
[25]朱慧,赵志红,施文蓉.应用单磺酰氯柱前衍生法测定食品中的牛磺酸[J].食品科学,2000,21(12):116-118
[26]WOOLLARD D C,INDYK H E.Taurine analysis in milk and infant formulae by liquid chromatography:collaborative study[J].Journal of Aoac International,1997,80(4):860-865
[27]BIONDI P A,MANCA F,NEGRI A.HPLC determination of plasma taurine[J].Chromatographia,1987,24(1):360-362
[28]中华人民共和国国家卫生和计划生育委员会.食品安全国家标准食品中牛磺酸的测定:GB5009.169-2016[S].北京:中国标准出版社,2017
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