干旱区生态环境知识资源中心(Arid): 超高效合相色谱法拆分和测定婴幼儿配方乳粉中肉碱对映体

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	超高效合相色谱法拆分和测定婴幼儿配方乳粉中肉碱对映体
其他题名	Chiral Separation and Determination of Carnitine Enantiomers in Infant Formula by Ultra-Performance Convergence Chromatography
	张文华; 谢文; 侯建波; 张雅琴; 汪鹏; 胡晓莉; 徐敦明
来源期刊	理化检验. B, 化学分册
ISSN	1001-4020
出版年	2021
卷号	57 期号:11 页码:970-976
中文摘要	建立了超高效合相色谱法(UPC2)拆分和测定婴幼儿配方乳粉中两种肉碱对映体(D-肉碱和L-肉碱)的方法。样品经0.1mol·L~(-1)盐酸溶液超声提取5min后,用1mol·L~(-1)氢氧化钾溶液在60℃水浴中皂化30min,离心,上清液在活化好的Oasis MCX型混合型强阳离子交换固相萃取柱上用含4%(体积分数)氨水的甲醇溶液洗脱。洗脱液经氮吹至近干,用含L-丙氨酸-beta-萘胺的乙腈溶液在催化剂的作用下于20℃静置衍生60min,离心、浓缩、过滤后,滤液中的目标物在Acquity Trefoil CEL1手性色谱柱上以不同体积比的超临界二氧化碳和含1%(体积分数)氨水的甲醇溶液组成的混合溶液为流动相进行梯度洗脱。结果表明,方法可以有效拆分肉碱外消旋体,两种肉碱对映体均在0.25~10.00mg·L~(-1)内与其对应的峰面积呈线性关系,测定下限(10S/N)均为25mg·kg~(-1);对空白样品进行3个浓度水平的加标回收试验,回收率为93.0%~110%,测定值的相对标准偏差(n=6)为3.9%~5.5%;方法用于20个实际样品的分析,未检出D-肉碱,而L-肉碱测定值满足GB 28050-2011和GB 13432-2013的要求,且方法与GB 29989-2013中的分光光度法无显著性差异。
英文摘要	A method for chiral separation and determination of 2carnitine enantiomers(D-carnitine and Lcarnitine) in infant formula by ultra-performance convergence chromatography(UPC2)was established.Samples were extracted by ultrasound with 0.1mol·L~(-1) hydrochloric acid solution for 5min,and saponified with 1mol·L~(-1) potassium hydroxide solution in a water bath at 60℃for 30min.The supernatant obtained by centrifugation was purified on an activated Oasis MCX type mixed strong cation exchange solid phase extraction column,and eluted with methanol solution containing 4% (phi)ammonium hydroxide.The eluate was blown to near dryness with nitrogen and derivatized with acetonitrile solution containing L-alanine-beta-naphthylamine in the presence of catalyst at 20℃for 60min.After centrifugation,concentration and filtration,the targets in the filtrate were subjected to gradient elution on an Acquity Trefoil CEL1chiral column with mobile phases composed of supercritical carbon dioxide and methanol solution containing 1% (phi)ammonium hydroxide ammonium hydroxide at different volume ratios.The results showed that the method could effectively separate carnitine racemates,and linear relationships between mass concentrations of two carnitine enantiomers and their corresponding peak areas were kept in the range of 0.25-10.00mg·L~(-1),with the same lower limit of determination(10S/N)of 25mg·kg~(-1).Test for spiked recovery was made on the blank samples at 3concentration levels,giving results of recovery in the range of 93.0%-110%,with RSDs(n=6)of the determined values in the range of 3.9%-5.5%.The proposed method was used for the analysis of 20actual samples,and no D-carnitine was detected,while the determined values of Lcarnitine met the requirements of GB 28050-2011and GB 13432-2013,and there was no significant difference between the prescribed method and the spectrophotometric method of GB 29989-2013.
中文关键词	超高效合相色谱法 ; 肉碱对映体 ; 拆分 ; 测定 ; 婴幼儿配方乳粉
英文关键词	ultra-performance convergence chromatography carnitine enantiomer chiral separation determination infant formula
类型	Article
语种	中文
收录类别	CSCD
WOS类目	Chemistry
CSCD记录号	CSCD:7104211
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/377772
作者单位	张文华, 杭州海关技术中心;;浙江省检验检疫科学技术研究院, ;;, 杭州;;杭州, ;; 310016;;310016.; 谢文, 杭州海关技术中心;;浙江省检验检疫科学技术研究院, ;;, 杭州;;杭州, ;; 310016;;310016.; 侯建波, 杭州海关技术中心;;浙江省检验检疫科学技术研究院, ;;, 杭州;;杭州, ;; 310016;;310016.; 张雅琴, 浙江省检验检疫科学技术研究院, 杭州, 浙江 310016, 中国.; 汪鹏, 浙江省检验检疫科学技术研究院, 杭州, 浙江 310016, 中国.; 胡晓莉, 浙江省检验检疫科学技术研究院, 杭州, 浙江 310016, 中国.; 徐敦明, 厦门海关技术中心, 厦门, 福建 361026, 中国.
推荐引用方式 GB/T 7714	张文华,谢文,侯建波,等. 超高效合相色谱法拆分和测定婴幼儿配方乳粉中肉碱对映体[J],2021,57(11):970-976.
APA	张文华.,谢文.,侯建波.,张雅琴.,汪鹏.,...&徐敦明.(2021).超高效合相色谱法拆分和测定婴幼儿配方乳粉中肉碱对映体.理化检验. B, 化学分册,57(11),970-976.
MLA	张文华,et al."超高效合相色谱法拆分和测定婴幼儿配方乳粉中肉碱对映体".理化检验. B, 化学分册 57.11(2021):970-976.