基于超高效合相色谱技术的保健食品中肉碱对映体拆分和测定方法研究  

Research on Separation and Determination of Carnitine Enantiomers in Health Foods Based on Ultra-performance Convergence Chromatography

作　　者：张文华 谢文 侯建波 汪鹏 徐敦明 姚滨滨 何建敏 严颖鹏 ZHANG Wen-hua;XIE Wen;HOU Jian-bo;WANG Peng;XU Dun-ming;YAO Bin-bin;HE Jian-min;YAN Ying-peng(Technical Center of Hangzhou Customs,Hangzhou 310016,China;Zhejiang Academy of Science and Technology for Inspection and Quarantine,Hangzhou 310016,China;Technical Center of Xiamen Customs,Xiamen 361026,China)

机构地区：[1]杭州海关技术中心,浙江杭州310016 [2]浙江省检验检疫科学技术研究院,浙江杭州310016 [3]厦门海关技术中心,福建厦门361026

出　　处：《分析测试学报》2021年第12期1713-1719,共7页Journal of Instrumental Analysis

基　　金：海关总署科研项目(2020HK196);浙江省科技计划项目(2018C37014)。

摘　　要：建立了一种超高效合相色谱(UPC2)拆分肉碱对映体及测定其在保健食品中含量的分析方法。试样经无水乙醇超声提取,提取液经衍生化后,采用Acquity Trefoil CEL1手性色谱柱(3.0 mm×150 mm,2.5μm)分离,以超临界CO2和氨水甲醇溶液(1∶99,体积比)为流动相梯度洗脱,2种肉碱对映体的分离效果最好。结果表明,右旋肉碱(D-肉碱)和左旋肉碱(L-肉碱)在0.50~20.00 mg/L范围内线性良好,相关系数(r2)大于0.999,方法定量下限(S/N=10)均为25 mg/kg;3个加标水平下的回收率为86.0%~110%,相对标准偏差(RSD)为4.3%~7.0%。应用该方法测定10份市售保健食品中D-肉碱和L-肉碱的含量,结果显示,10份保健食品中均未检出D-肉碱,检出L-肉碱的含量均达到标签值的96%~102%。该方法具有分析速度快、分离效果好、重现性好、有机溶剂用量少等特点,可为手性药物开发、使用及相关法规的制定提供科学支撑。Separation of two carnitine enantiomers,i.e.D-carnitine and L-carnitine by ultra-performance convergence chromatography(UPC2)was attempted,and a residue analytical method for these carnitine enantiomers in health food samples was established.The solid and liquid health food samples were ultrasonically extracted with ethyl alcohol as the solvent.After derivatization of the extracting solution,a chiral chromatographic column,Acquity Trefoil CEL1(3.0 mm×150 mm,2.5μm)column was adopted for separation.The detection wavelenths for photo-diode array detector(PAD)was 244 nm.The separation effect of the two carnitine enantiomers reached the best when supercritical carbon dioxide and ammonium hydroxide-methanol(1∶99,by volume)were taken as the mobile phases at a flow rate of 1.0 mL/min by gradient elution.Results showed that there were good linear relationships for the two carnitine enantiomers in the range of 0.50-20.00 mg/L,with correlation coefficients(r^(2))greater than 0.999.The quantitative limits of the method(S/N=10)for D-carnitine and L-carnitine were both 25 mg/kg.Recovery experiment was carried out within the range of 25-250 mg/kg,and the recoveries at three spiked levels ranged from 86.0%to 110%,with the relative standard deviations(RSD)of 4.3%-7.0%.The method was used to detect standard carnitine racemates purchased from the reagent company in order to investigate its effectiveness and practicability.The results suggested that D-carnitine accounted for 51.2%and L-carnitine accounted for 48.8%in the standard carnitine racemates.This method was also used to detect the contents of D-carnitine and L-carnitine in 10 health foods purchased from the market.The experimental results indicated that D-carnitine wasn't detected in the 10 health food samples,but L-carnitine was detected in all of them,with the content reaching 96%-102%of the label value.With the characteristics of rapid analysis,good separation effect,good reproducibility and low consumption of organic solvent,this method is applicable for both the det

关 键 词：超高效合相色谱 肉碱 保健食品 对映体 手性分离 

分 类 号：O657.7[理学—分析化学] TS207.3[理学—化学]