超高效液相色谱法同时测定含乳饮料中12种食品添加剂
|
摘要
目的建立超高效液相色谱法同时快速测定含乳饮料中3种甜味剂、7种防腐剂和2种酸味剂的检测方法。方法样品用水提取后,加入亚铁氢化钾和乙酸锌溶液沉淀蛋白质及其他杂质。以Waters XBridge BEHC18柱(100mm×2.1mm,i.d.1.7μm)为分离柱,甲醇-20mmol/L乙酸铵溶液为流动相梯度洗脱,流速为0.3 mL/min,采用二极管阵列检测器进行检测,检测波长为230 nm和210 nm。结果 12种目标物可以在6 min内达到较好的分离,在0.010～80μg/mL范围内呈良好的线性关系(r2≥0.9996),检出限为0.03～0.15 mg/kg,定量限0.10～0.50mg/kg,样品在3个加标水平(1、10和50mg/kg)的回收率为80.2%～99.7%,相对标准偏差为1.23%～4.70%。结论该方法操作简单,快速,适用于含乳饮料中12种食品添加剂的检测。
Objective To establish a method for simultaneous determination of 3 kinds of preservatives, 7 kinds of sweeteners and 2 kinds of acidulants in milk-containing beverage by ultra performance liquid chromatography(UPLC). Methods After the sample was extracted with water, ferrous potassium hydride and zinc acetate solution were added to precipitate proteins and other impurities, and then it was gradient eluted by a column of Waters XBridge BEH C_(18)(100 mm×2.1 mm, i.d. 1.7 μm) with the mobile phase of methanol and 20 mmol/L ammonium acetate solution at a flow rate of 0.3 mL/min. Detection was performed using a diode array detector with detection wavelengths of 230 nm and 210 nm. Results The 12 kinds of food additives could be effectively separated within 6 min. In the range of 0.010-80 μg/mL, there was a good linear relationship(r2≥0.9996), the limit of detection was 0.03-0.15 mg/kg, and the limit of quantification was 0.10-0.50 mg/kg. The recoveries of samples at 3 levels(1, 10 and 50 mg/kg) were 80.2%-99.7% and the relative standard deviations(RSDs) were 1.23%-4.70%. Conclusion This method is rapid and convenient, which is suitable for the determination of 12 kinds of food additives in milk-containing beverages.
Objective To establish a method for simultaneous determination of 3 kinds of preservatives, 7 kinds of sweeteners and 2 kinds of acidulants in milk-containing beverage by ultra performance liquid chromatography(UPLC). Methods After the sample was extracted with water, ferrous potassium hydride and zinc acetate solution were added to precipitate proteins and other impurities, and then it was gradient eluted by a column of Waters XBridge BEH C_(18)(100 mm×2.1 mm, i.d. 1.7 μm) with the mobile phase of methanol and 20 mmol/L ammonium acetate solution at a flow rate of 0.3 mL/min. Detection was performed using a diode array detector with detection wavelengths of 230 nm and 210 nm. Results The 12 kinds of food additives could be effectively separated within 6 min. In the range of 0.010-80 μg/mL, there was a good linear relationship(r2≥0.9996), the limit of detection was 0.03-0.15 mg/kg, and the limit of quantification was 0.10-0.50 mg/kg. The recoveries of samples at 3 levels(1, 10 and 50 mg/kg) were 80.2%-99.7% and the relative standard deviations(RSDs) were 1.23%-4.70%. Conclusion This method is rapid and convenient, which is suitable for the determination of 12 kinds of food additives in milk-containing beverages.
引文
[1]GB/T 21732-2008食品安全国家标准含乳饮料[S].GB/T 21732-2008 National food safety standard-Milk beverage[S].
[2]刘印平,路杨,杨立新,等.超高效液相色谱-串联质谱法快速测定饮料中22种添加剂[J].食品安全质量检测学报,2015,(3):980-986.Liu YP,Lu Y,Yang LX,et al.Simultaneous determination of 22 additives in beverage by ultra performance liquid chromatography-tandem mass spectrometry[J].J Food Saf Qual,2015,(3):980-986.
[3]Tfouni SAV,Toledo MCF.Determination of benzoic and sorbic acids in Brazilian food[J].Food Control,2002,13(2):117-123.
[4]Golden R,Gandy J,Vollmer G.A review of the endocrine activity of parabens and implications for potential risks to human health[J].Crit Rev Toxicol,2005,35(5):435-458.
[5]吕冰峰,吕卓,应雨晴,等.2016~2017年全国食品安全监督抽检结果分析[J].食品安全质量检测学报,2018,9(11):2862-2867.Lv BF,Lv Z,Ying YQ,et al.National food supervision and sampling inspection in 2016-2017[J].J Food Saf Qual,2018,9(11):2862-2867.
[6]GB 5009.28-2016食品安全国家标准食品中苯甲酸、山梨酸和糖精钠的测定[S].GB5009.28-2016 National food safety standard-Determination of benzonic acid,sorbic acid and saccharin sodium in food[S].
[7]GB 5009.121-2016食品安全国家标准食品中脱氢乙酸的测定[S].GB 5009.121-2016 National food safety standard-Determination of dehydroacetic acid in food[S].
[8]GB 5009.263-2016食品安全国家标准食品中阿斯巴甜和阿力甜的测定[S].GB 5009.263-2016 National food safety standard-Determination of aspartame and altanle in food[S].
[9]蒋孟圆,张瑞雨,刘晓松,等.二级管阵列-超快速液相色谱法同时测定食品中5种添加剂的含量[J].食品安全质量检测学报,2017,8(10):3819-3825.Jiang MY,Zhang RY,Liu XS,et al.Simultaneous determination of 5 kinds of additives in food by ultra high performance liquid chromatography with diode array detector[J].J Food Saf Qual,2017,8(10):3819-3825.
[10]牟宵,张璐,张崇淼,等.超高效液相色谱法同时测定饮料中14种食品添加剂[J].食品安全质量检测学报,2017,8(8):3177-3184.Mou X,Zhang L,Zhang CM,et al.Simultaneous determination of 14kinds of food additives in beverage by ultra performance liquid chromatography[J].J Food Saf Qual,2017,8(8):3177-3184.
[11]谭建林,冯雷,俸金梅,等.高效液相色谱法同时测定食品中12种防腐剂和甜味剂[J].食品安全质量检测学报,2016,7(10):4101-4105.Tan JL,Feng L,Feng JM,et al.Simultaneous determination of 12 kinds of preservatives and sweeteners in food by high performance liquid chromatography[J].J Food Saf Qual,2016,7(10):4101-4105.
[12]卫星华,李荣,董曼曼,等.高效液相法同时测定饮品中8种食品添加剂[J].食品研究与开发,2017,38(24):137-140.Wei XH,Li R,Dong MM,et al.Determination of eight food additives in drink by HPLC[J].Food Res Dev,2017,38(24):137-140.
[13]Fabio F,Chiara G,Alessandro LM.Multi-detection of preservatives in cheeses by liquid chromatography-tandem mass spectrometry[J].JChromatogr B,2012,906(1):9-18.
[14]Xiu Q,Zhang LF,Sun YY,et al.Accurate screening for synthetic preservatives in beverage using high performance liquid chromatography with time-of-flight mass spectrometry[J].Anal Chim Acta,2008,608(2):165-177.
[15]Anton K.Analysis of a variety of inorganic and organic additives in food products by ion-pairing liquid chromatography coupled to high-resolution mass spectrometry[J].Anal Bioanal Chem,2018,410(22):5629-5640.
[16]周家萍,李典,李治东,等.气相色谱法同时测定食品中8种防腐剂[J].食品研究与开发,2017,38(14):161-163.Zhou JP,Li D,Li ZD,et al.Determination of eight food additives in drink by HPLC[J].Food Res Dev,2017,38(14):161-163.
[17]沈燕飞,朱仙娜,姚澄,等.阀切换离子色谱技术同时检测饮料中的糖类、甜味剂和防腐剂[J].食品科学,2018,39(16):311-315.Shen YF,Zhu XN,Yao C,et al.Simultaneous determination of sugarsedulcorant,and preservatives in beverages using ion chromatography couple of valve switching technique[J].Food Sci,2018,39(16):311-315.
[18]Souza DJFF,Guadalupe CA,Laís DAP,et al.Simple and fast method for simultaneous determination of propionate and sorbate in bread by capillary electrophoresis with UV spectrophotometric detection[J].J Food Compos Anal,2018,(72):93-96.
[19]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 uses of food additives[S].
[2]刘印平,路杨,杨立新,等.超高效液相色谱-串联质谱法快速测定饮料中22种添加剂[J].食品安全质量检测学报,2015,(3):980-986.Liu YP,Lu Y,Yang LX,et al.Simultaneous determination of 22 additives in beverage by ultra performance liquid chromatography-tandem mass spectrometry[J].J Food Saf Qual,2015,(3):980-986.
[3]Tfouni SAV,Toledo MCF.Determination of benzoic and sorbic acids in Brazilian food[J].Food Control,2002,13(2):117-123.
[4]Golden R,Gandy J,Vollmer G.A review of the endocrine activity of parabens and implications for potential risks to human health[J].Crit Rev Toxicol,2005,35(5):435-458.
[5]吕冰峰,吕卓,应雨晴,等.2016~2017年全国食品安全监督抽检结果分析[J].食品安全质量检测学报,2018,9(11):2862-2867.Lv BF,Lv Z,Ying YQ,et al.National food supervision and sampling inspection in 2016-2017[J].J Food Saf Qual,2018,9(11):2862-2867.
[6]GB 5009.28-2016食品安全国家标准食品中苯甲酸、山梨酸和糖精钠的测定[S].GB5009.28-2016 National food safety standard-Determination of benzonic acid,sorbic acid and saccharin sodium in food[S].
[7]GB 5009.121-2016食品安全国家标准食品中脱氢乙酸的测定[S].GB 5009.121-2016 National food safety standard-Determination of dehydroacetic acid in food[S].
[8]GB 5009.263-2016食品安全国家标准食品中阿斯巴甜和阿力甜的测定[S].GB 5009.263-2016 National food safety standard-Determination of aspartame and altanle in food[S].
[9]蒋孟圆,张瑞雨,刘晓松,等.二级管阵列-超快速液相色谱法同时测定食品中5种添加剂的含量[J].食品安全质量检测学报,2017,8(10):3819-3825.Jiang MY,Zhang RY,Liu XS,et al.Simultaneous determination of 5 kinds of additives in food by ultra high performance liquid chromatography with diode array detector[J].J Food Saf Qual,2017,8(10):3819-3825.
[10]牟宵,张璐,张崇淼,等.超高效液相色谱法同时测定饮料中14种食品添加剂[J].食品安全质量检测学报,2017,8(8):3177-3184.Mou X,Zhang L,Zhang CM,et al.Simultaneous determination of 14kinds of food additives in beverage by ultra performance liquid chromatography[J].J Food Saf Qual,2017,8(8):3177-3184.
[11]谭建林,冯雷,俸金梅,等.高效液相色谱法同时测定食品中12种防腐剂和甜味剂[J].食品安全质量检测学报,2016,7(10):4101-4105.Tan JL,Feng L,Feng JM,et al.Simultaneous determination of 12 kinds of preservatives and sweeteners in food by high performance liquid chromatography[J].J Food Saf Qual,2016,7(10):4101-4105.
[12]卫星华,李荣,董曼曼,等.高效液相法同时测定饮品中8种食品添加剂[J].食品研究与开发,2017,38(24):137-140.Wei XH,Li R,Dong MM,et al.Determination of eight food additives in drink by HPLC[J].Food Res Dev,2017,38(24):137-140.
[13]Fabio F,Chiara G,Alessandro LM.Multi-detection of preservatives in cheeses by liquid chromatography-tandem mass spectrometry[J].JChromatogr B,2012,906(1):9-18.
[14]Xiu Q,Zhang LF,Sun YY,et al.Accurate screening for synthetic preservatives in beverage using high performance liquid chromatography with time-of-flight mass spectrometry[J].Anal Chim Acta,2008,608(2):165-177.
[15]Anton K.Analysis of a variety of inorganic and organic additives in food products by ion-pairing liquid chromatography coupled to high-resolution mass spectrometry[J].Anal Bioanal Chem,2018,410(22):5629-5640.
[16]周家萍,李典,李治东,等.气相色谱法同时测定食品中8种防腐剂[J].食品研究与开发,2017,38(14):161-163.Zhou JP,Li D,Li ZD,et al.Determination of eight food additives in drink by HPLC[J].Food Res Dev,2017,38(14):161-163.
[17]沈燕飞,朱仙娜,姚澄,等.阀切换离子色谱技术同时检测饮料中的糖类、甜味剂和防腐剂[J].食品科学,2018,39(16):311-315.Shen YF,Zhu XN,Yao C,et al.Simultaneous determination of sugarsedulcorant,and preservatives in beverages using ion chromatography couple of valve switching technique[J].Food Sci,2018,39(16):311-315.
[18]Souza DJFF,Guadalupe CA,Laís DAP,et al.Simple and fast method for simultaneous determination of propionate and sorbate in bread by capillary electrophoresis with UV spectrophotometric detection[J].J Food Compos Anal,2018,(72):93-96.
[19]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 uses of food additives[S].