Optimization of the National Standard Method for the Determination of Antioxidants in Edible Oils by High Performance Liquid Chromatography
摘 要
对国家标准GB 5009.32-2016中测定食品中抗氧化剂的高效液相色谱法进行了优化。优化的试验条件如下:样品用乙腈饱和的正己烷溶液溶解,再用含L-抗坏血酸棕榈酸酯的正己烷饱和的乙腈溶液提取(10 mL×3);采用C18固相萃取柱净化;以Agilent Eclipse XDB-C18色谱柱(250 mm×4.6 mm,5 μm)为固定相,以不同体积比的0.1%(体积分数)甲酸溶液-乙腈混合液为流动相进行梯度洗脱。优化结果表明:9种抗氧化剂在30 min内完全分离,峰形对称,分离度较好,解决了国家标准方法中没食子酸丙酯(PG)峰形较差、2,4,5-三羟基苯丁酮(THBP)和叔丁基对苯二酚(TBHQ)未能达到基线分离等问题;加标回收率由标准方法的31.4%~90.1%提高至62.0%~104%,测定值的相对标准偏差(n=6)均小于13%。
Abstract
A method of high performance liquid chromatography for the determination of antioxidants in food in the national standard GB 5009.32-2016 was optimized. The optimized test conditions were as follows: Samples were dissolved in n-hexane saturated with acetonitrile, and the antioxidants were extracted 3 times by 10 mL of acetonitrile saturated with n-hexane (containing Ascorbyl Palmitate); the C18 solid phase extraction column was used for purification. The Agilent Eclipse XDB-C18 column (250 mm×4.6 mm, 5 μm) was used as stationary phase, and 0.1% (volume fraction) formic acid-acetonitrile mixtures in different volume ratios were used as mobile phase for gradient elution. The optimized results showed that the 9 antioxidants were completely separated within 30 min, the peak shapes were symmetrical, and the resolution was better, which solved the problems including the poor peak shape of PG and the failure of the baseline separation of THBP and TBHQ in the national standard method. The spiked recovery increased from 31.4%-90.1% of the national standard method to 62.0%-104%, and RSDs (n=6) of the determined values were all less than 13%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202106007
所属栏目 工作简报
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收稿日期 2020/11/28
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备注钟慈平,工程师,硕士,研究方向为食品理化检测
引用该论文: ZHONG Ciping,CHENG Changyu,SU Xin,ZHOU Haiyan,MA Wei,YU Xiaoqin. Optimization of the National Standard Method for the Determination of Antioxidants in Edible Oils by High Performance Liquid Chromatography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(6): 519~525
钟慈平,成长玉,苏欣,周海燕,马伟,余晓琴. 高效液相色谱法测定食用油中抗氧化剂的国家标准方法的优化研究[J]. 理化检验-化学分册, 2021, 57(6): 519~525
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【8】辛丽娜,刘常凯,何林飞.HPLC法同时测定月饼中9种抗氧化剂的研究方法[J].中国食品添加剂, 2019,30(9):176-181.
【9】MACARI E R, SCHAEFFER E K, WEST R J, et al. Simvastatin and t-butylhydroquinone suppress KLF1 and BCL11A gene expression and additively increase fetal hemoglobin in primary human erythroid cells[J]. Blood, 2013,121(5):830-839.
【10】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添加剂使用标准:GB 2760-2014[S].北京:中国标准出版社, 2015.
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【12】杨卫花,徐幸,赵浩军,等.气相色谱/三重串联四极杆质谱分析食用植物油中抗氧化剂BHA、BHT和TBHQ[J].粮食储藏, 2013,42(1):41-44.
【13】蔡发,段小娟,牟志春,等.高效液相色谱法同时测定食品中的12种抗氧化剂[J].食品科学, 2010,31(8):207-211.
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