L-苯丙氨酸纯度及其杂质分析方法的研究  

Chemical Purity and Impurities of L-Phenylalanine

作　　者：刘照[1] 暴海霞[1,2] 戴新华[1] 张伟[1] 李孟婉 

机构地区：[1]中国计量科学研究院化学计量与分析科学研究所,北京100013 [2]苏州市计量测试研究所,苏州215128

出　　处：《化学试剂》2015年第12期1057-1062,1101,共7页Chemical Reagents

基　　金：国家科技基础专项"心血管与肿瘤疾病诊断重要标志物标准物质的研究"资助项目(2011FY130100);国家科技支撑计划课题"有机纯物质高准确度化学计量溯源技术研究"资助项目(2013BAK10B01)

摘　　要：L-苯丙氨酸是人体必需氨基酸之一,广泛应用于医药、食品、化妆品和临床检验等领域。主要通过采用高效液相色谱-电喷雾检测法(HPLC-CAD)和高效液相色谱串联三重四极质谱法(HPLC-MS/MS)对与主成分结构类似的杂质进行了定性和定量分析。另外,对L-和D-苯丙氨酸进行分离和定量分析;采用顶空进样与气相色谱氢火焰离子化检测器(FID)联用法对易挥发性杂质(VOCs)进行了定性和定量分析;采用卡尔费休库仑法对水分进行测定,同时采用热重(TGA)法进行验证;采用电感耦合等离子体质谱法(ICP-MS)对不挥发性杂质进行分析,采用灼烧残渣法进行了验证。在上述杂质分析的基础上,同时采用质量平衡法和定量核磁法对L-苯丙氨酸纯度进行定值,并对测量不确定度进行了评定,最终得到L-苯丙氨酸的纯度值为994.31(±3.96)mg/g。L-Phenylalanine is one of the indispensable amino acid,which is widely used in medicine,food,cosmetics,clinical analysis and other industries. In this work,the methods of HPLC-CAD and HPLC-MS / MS were applied for the qualitative and quantitative analysis of the related structure impurities. Moreover,an HPLC method using chiral column was used to isolate and analyze L-and D-phenylalanine. The residual organic solvents（ VOCs） were analyzed using headspace gas chromatography. The water content was determined using Karl Fischer coulometric method and confirmed by thermogravimetry（ TGA） method. The content of the non-volatiles / inorganics was carried out by inductively coupled plasma mass spectroscopy（ ICP-MS） and verified by ash residue method. Using the above impurity analysis as a foundation,both mass balance method and quantitative NMR method were employed to certify the purity property value. The uncertainty of the above four kinds impurities was evaluated by the comprehensive analysis the various influencing factors. Finally,the purity of L-phenylalanine sample is 994. 31（ ± 3. 96） mg / g.

关 键 词：L-苯丙氨酸 纯度 杂质 HPLC-MS/MS 质量平衡法 定量核磁法 

分 类 号：O657[理学—分析化学]