高效液相色谱法测定食用植物油中6种合成抗氧化剂
|
摘要
建立高效液相色谱法测定食用植物油中没食子酸丙酯、叔丁基对苯二酚、叔丁基对羟基茴香醚、二丁基羟基甲苯、没食子酸、山梨酸6种合成类抗氧化剂的含量。样品经正己烷溶解,再用饱和正己烷的乙腈萃取,振荡,超声25 min,离心后取乙腈层,定容,过0.45μm滤膜。以0.4%乙酸水溶液–乙腈为流动相,流量为0.8 mL/min,梯度洗脱,检测波长为280 nm,采用高效液相色谱法进行检测。6种合成抗氧化剂的质量浓度在0.1～10μg/mL范围内与色谱峰面积呈良好的线性关系,相关系数均大于0.999,方法检出限均为1.0～2.5 mg/kg。样品的加标回收率为79.6%～108.9%,测定结果的相对标准偏差为2.03%～5.77%(n=6)。该方法操作简单,能同时检测6种合成抗氧化剂,适用于多种食用植物油中合成抗氧化剂的测定。
A method for the determination of propyl gallate(PG), tertiary butylhydroquinone(TBHQ), butylated hyd-roxylanisole(BHA), butylated hyd-roxytoluene(BHT), gallic acid and sorbic acid in edible vegetable oil by high performance liquid chromatography was established. The samples were dissolved in n-hexane, then extracted with saturated n-hexane acetonitrile, oscillated, ultrasound for 25 minutes, centrifuged, acetonitrile layer was taken, through 0.45 μm?lter membrane after constant volume. The mobile phase was 0.4% acetic acid aqueous solution – acetonitrile, ?ow rate was 0.8 mL/min, gradient elution, detection wavelength was 280 nm, and the detection was carried out by high performance liquid chromatography. The mass concentration of six synthetic antioxidants in the range of 0.1–10 μg/mL showed good linear relationships with the peak area, the correlation coef?cients were more than 0.999, and the detection limits were1.0–2.5 mg/kg. The recoveries of the samples were 79.6%–108.9%, and the relative standard deviations of the results were2.03%–5.77%(n=6). The method is simple and it can simultaneously detect six synthetic antioxidants. It is suitable for the determination of synthetic antioxidants in various edible vegetable oils.
A method for the determination of propyl gallate(PG), tertiary butylhydroquinone(TBHQ), butylated hyd-roxylanisole(BHA), butylated hyd-roxytoluene(BHT), gallic acid and sorbic acid in edible vegetable oil by high performance liquid chromatography was established. The samples were dissolved in n-hexane, then extracted with saturated n-hexane acetonitrile, oscillated, ultrasound for 25 minutes, centrifuged, acetonitrile layer was taken, through 0.45 μm?lter membrane after constant volume. The mobile phase was 0.4% acetic acid aqueous solution – acetonitrile, ?ow rate was 0.8 mL/min, gradient elution, detection wavelength was 280 nm, and the detection was carried out by high performance liquid chromatography. The mass concentration of six synthetic antioxidants in the range of 0.1–10 μg/mL showed good linear relationships with the peak area, the correlation coef?cients were more than 0.999, and the detection limits were1.0–2.5 mg/kg. The recoveries of the samples were 79.6%–108.9%, and the relative standard deviations of the results were2.03%–5.77%(n=6). The method is simple and it can simultaneously detect six synthetic antioxidants. It is suitable for the determination of synthetic antioxidants in various edible vegetable oils.
引文
[1]NATALY A S,SARAH S D,PEDRO H M D A,et al.Effects of added Phenolics on the storage stability of avocado and coconut oils[J].Energy&fuels,2011,25:4 190-4 194.
[2]REZA F,MOHAMMAD H T K.Polar compounds distribution of sunflower oil as affected by unsaponifiable matters of bene hull oil(BHO)and tertiary-butylhydroquinone(TBHQ)during deep-frying[J].Food chemistry,2010,122:381-385.
[3]BURCU B,MUSTAFA?,KUBILAY G,et al.Tert-butylhydroquinone as a spectroscopic probe for the superoxide radical scavenging activity assay of biological samples[J].Analytical chemistry,2011,83:5 652-5 660.
[4]郝鹏鹏,倪晋仁,孙卫玲.叔丁基对苯二酚两种代谢物的代谢动力学[J].食品科学,2012,33(3):220-224.
[5]徐歆,毛予龙,黄琴,等.特丁基对苯二酚对高脂日粮小鼠抗氧化功能的影响[J].营养学报,2012,34(1):89-91.
[6]GB 5009.32-2016食品安全国家标准食品中9种抗氧化剂的测定[S].
[7]杨小兵,丁松涛,王安邦.特丁基对苯二酚的电子轰击质谱研究[J].质谱学报,2011,32(5):278-282.
[8]郝媛媛,丁轶聪,张岩岩.HPLC-UV法测定食品中抗氧化剂特丁基对苯二酚(TBHQ)[J].中国卫生检验杂志,2010,20(4):748-749.
[9]HUANG W,NIU H,SHI B,et al.HPLC coupled with ion trap MS/MS for analysis of tertiary butylhydroquinone in edible oil samples[J].Journal of food lipids,2008,(15):1-12.
[10]HUANG W,GU Y C,NIU H.Determination of tertiarybutylhydroquinone and its metabolites in rat serum by liquid chromatography-ion trap mass spectrometry[J].Lipids,2008(43):281-288.
[11]周相娟,赵玉琪,李伟,等.气相色谱/质谱法检测食品塑料包装材料中三种抗氧剂[J].食品工业科技,2010,31(9):288-290.
[12]魏树龙,寇立娟,梁春实,等.气相色谱-质谱联用法测定植物油和鸡肉中抗氧化剂BHA BHT和TBHQ[J].农产品加工学刊,2011(10):101-104.
[13]张曼,蔡禾,沈京玲.食品添加剂特丁基对苯二酚的太赫兹光谱及其检测分析[J].光谱学与光谱分析,2011,31(7):1 809-1 813.
[14]GB/T 23495-2009食品中苯甲酸、山梨酸和糖精钠的测定高效液相色谱法[S].
[15]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].
[16]陈俊,黄琼,邹萍,等.HPLC法同时测定四川泡菜中苯甲酸、山梨酸、柠檬黄和姜黄[J].中国调味品,2010,35(12):104-106.
[2]REZA F,MOHAMMAD H T K.Polar compounds distribution of sunflower oil as affected by unsaponifiable matters of bene hull oil(BHO)and tertiary-butylhydroquinone(TBHQ)during deep-frying[J].Food chemistry,2010,122:381-385.
[3]BURCU B,MUSTAFA?,KUBILAY G,et al.Tert-butylhydroquinone as a spectroscopic probe for the superoxide radical scavenging activity assay of biological samples[J].Analytical chemistry,2011,83:5 652-5 660.
[4]郝鹏鹏,倪晋仁,孙卫玲.叔丁基对苯二酚两种代谢物的代谢动力学[J].食品科学,2012,33(3):220-224.
[5]徐歆,毛予龙,黄琴,等.特丁基对苯二酚对高脂日粮小鼠抗氧化功能的影响[J].营养学报,2012,34(1):89-91.
[6]GB 5009.32-2016食品安全国家标准食品中9种抗氧化剂的测定[S].
[7]杨小兵,丁松涛,王安邦.特丁基对苯二酚的电子轰击质谱研究[J].质谱学报,2011,32(5):278-282.
[8]郝媛媛,丁轶聪,张岩岩.HPLC-UV法测定食品中抗氧化剂特丁基对苯二酚(TBHQ)[J].中国卫生检验杂志,2010,20(4):748-749.
[9]HUANG W,NIU H,SHI B,et al.HPLC coupled with ion trap MS/MS for analysis of tertiary butylhydroquinone in edible oil samples[J].Journal of food lipids,2008,(15):1-12.
[10]HUANG W,GU Y C,NIU H.Determination of tertiarybutylhydroquinone and its metabolites in rat serum by liquid chromatography-ion trap mass spectrometry[J].Lipids,2008(43):281-288.
[11]周相娟,赵玉琪,李伟,等.气相色谱/质谱法检测食品塑料包装材料中三种抗氧剂[J].食品工业科技,2010,31(9):288-290.
[12]魏树龙,寇立娟,梁春实,等.气相色谱-质谱联用法测定植物油和鸡肉中抗氧化剂BHA BHT和TBHQ[J].农产品加工学刊,2011(10):101-104.
[13]张曼,蔡禾,沈京玲.食品添加剂特丁基对苯二酚的太赫兹光谱及其检测分析[J].光谱学与光谱分析,2011,31(7):1 809-1 813.
[14]GB/T 23495-2009食品中苯甲酸、山梨酸和糖精钠的测定高效液相色谱法[S].
[15]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].
[16]陈俊,黄琼,邹萍,等.HPLC法同时测定四川泡菜中苯甲酸、山梨酸、柠檬黄和姜黄[J].中国调味品,2010,35(12):104-106.
© 2004-2018 中国地质图书馆版权所有 京ICP备05064691号 京公网安备11010802017129号 地址：北京市海淀区学院路29号 邮编：100083 电话：办公室：(+86 10)66554848；文献借阅、咨询服务、科技查新：66554700 |