Improvement of National Standard Method for Determination of 16 Kinds of Amino Acids in Food
摘 要
对国家标准GB 5009.124-2016测定食品中16种氨基酸(天冬氨酸、苏氨酸、丝氨酸、谷氨酸、脯氨酸、甘氨酸、丙氨酸、缬氨酸、蛋氨酸、异亮氨酸、亮氨酸、酪氨酸、苯丙氨酸、组氨酸、赖氨酸、精氨酸)含量进行了方法改进。改进后的酸水解条件如下:称取样品1 g于聚四氟乙烯管中,加入含0.1%(质量分数)苯酚的6 mol·L-1盐酸溶液10 mL,充氮后封口,酸水解温度为165℃,酸水解时间由原来的22 h缩短至1 h。并提出了微波消解的前处理方法,其条件如下:称取样品约0.1 g于石英罐中,加入6 mol·L-1盐酸溶液1 mL,将其放进装有6 mol·L-1盐酸溶液的聚四氟乙烯罐中,充氮除氧,封盖后放入消解仪,微波消解温度为165℃,消解时间为12 min。以LCA K06/Na色谱柱为固定相,按照优化后的柱升温程序和梯度洗脱程序对16种氨基酸进行分离。结果表明:16种氨基酸的浓度在10~200 μmol·L-1内与其对应的峰面积呈线性关系,检出限为0.000 11%~0.004 2%;对猪瘦肉进行3个浓度水平的加标回收试验,16种氨基酸的回收率为93.6%~101%,测定值的相对标准偏差(RSD,n=6)为1.2%~7.2%;两种前处理方法用于实际样品的测定,并与GB 5009.124-2016的测定结果进行比对,P值分别为0.870和0.643,说明这两种前处理方法的测定结果与GB 5009.124-2016的不存在显著性差异。
Abstract
The national standard method GB 5009.124-2016 for determination of 16 kinds of amino acids (including of aspartic acid, threonine, serine, glutamic acid, proline, glycine, alanine, valine, methionine, isoleucine, leucine, tyrosine, phenylalanine, histidine, lysine, arginine) in food was improved. Improved conditions of acid hydrolysis were as following. Sample of 1 g was placed into a teflon tube, and 6 mol·L-1 hydrochloric acid solution containing 0.1% (mass fraction) phenol of 10 mL was added for filling nitrogen and sealing. The acid hydrolysis tempreture was 165℃ and the acid hydrolysis time was shortened to 1 h from 22 h. Microwave digestion was proposed, and the conditions were as following. Sample of 0.1 g was placed into a quartz tank, and 6 mol·L-1 hydrochloric acid solution of 1 mL was added. The above solution was put into a teflon tank containing 6 mol·L-1 hydrochloric acid solution and digested at 165℃ for 12 min after filling nitrogen for deoxygenation and sealing. LCA K06/Na column was used as stationary phase, and 16 kinds of amino acids were separated according to optimized column heating program and gradient elution program. It was showed that linear relationships between concentrations of 16 kinds of amino acids and their peak areas were kept in the range of 10-200 μmol·L-1, with detection limits in the range of 0.000 11%-0.004 2%. Recovery test was made on pig lean meat at 3 concentration levels by standard addition method, giving results in the range of 93.6%-101%, and RSDs (n=6) of the determined values were in the range of 1.2%-7.2%. The two pretreatment methods have been used for determination of substantial samples, and compared with the determination results of GB 5009.124-2016. Values of P were 0.870 for improved acid hydrolysis and 0.643 for microwave digestion, indicating that there was no significant difference between the determination results of these two pretreatment methods and GB 5009.124-2016.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202201013
所属栏目 工作简报
基金项目
收稿日期 2020/8/6
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备注李巧琪,工程师,本科,主要从事食品理化检验工作,493881592@qq.com
引用该论文: LI Qiaoqi,LI Hongyan,LU Guifeng,ZHOU Hailian,XU Zhibin. Improvement of National Standard Method for Determination of 16 Kinds of Amino Acids in Food[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2022, 58(1): 77~83
李巧琪,李洪燕,卢桂锋,周海练,许志彬. 测定食品中16种氨基酸国家标准方法的改进[J]. 理化检验-化学分册, 2022, 58(1): 77~83
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参考文献
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【3】国家卫生和计划生育委员会,国家食品药品监督管理总局.食品安全国家标准食品中氨基酸的测定:GB 5009.124-2016[S].北京:中国标准出版社, 2017.
【4】王忠合,李晓婷,胡文梅,等.超高压液相色谱-高分辨质谱法检测单丛乌龙茶中氨基酸[J].食品与发酵工业, 2020,46(21):207-214.
【5】王馨雨,王蓉蓉,王婷,等.不同品种百合内外鳞片游离氨基酸组成的主成分分析及聚类分析[J].食品科学, 2020,41(12):211-220.
【6】QIU X, REYNOLDS R, JOHANNINGSMEIER S, et al. Determination of free amino acids in five commercial sweetpotato cultivars by hydrophilic interaction liquid chromatography-mass spectrometry[J]. Journal of Food Composition and Analysis, 2020,92:103522.
【7】黄元河,潘乔丹,黎惠琴,等.柱前衍生-高效液相色谱法测定野芭蕉不同部位的18种氨基酸含量[J].食品研究与开发, 2020,41(9):158-162.
【8】唐翎,魏伟,赵勇.柱前衍生高效液相色谱测定猴头菌丝体中15种游离氨基酸的含量[J].中国药学杂志, 2017,52(21):1899-1902.
【9】温浩然,冀艳华,韩星,等.利用柱前在线衍生-高效液相色谱法测定培植牛黄及天然牛黄中18种氨基酸的含量[J].中国现代中药, 2020,22(2):231-236.
【10】宋卫得,杜利君,高尧华,等.积分脉冲安培检测-离子色谱法同时测定果汁中20种氨基酸[J].中国食品添加剂, 2019,30(8):132-138.
【11】严俊,徐柏杨,颜琳琦,等.L-8900氨基酸分析仪检测不同形态保健食品中牛磺酸含量[J].食品工业, 2019,40(11):341-344.
【12】SONG W, SU Z, HUI X, et al. Simultaneous determination of twenty amino acids and six carbohydrates in soy sauce by ion chromatography with integrated pulsed amperometric detection[J]. Chinese Journal of Chromatography, 2019,37(9):996-1003.
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