今日药学

2020, v.30(09) 620-624+633

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柱后衍生法测定鲜竹沥中氨基酸的含量
Determination of Amino Acids in Fresh Bamboo Sap by Post-column Derivatization Cation-exchange Chromatography

洪挺;赵雯;周志强;罗跃华;付辉政;
HONG Ting;ZHAO Wen;ZHOU Zhiqiang;LUO Yuehua;FU Huizheng;Jiangxi Provicial Institute for Drug and Food Control,Jiangxi Provincial Engineering Research Center for Drug and Medical Device Quality,NMPA Key Laboratory for Quality Evaluation of Traditional Chinese Medicine (Traditional Chinese Patent Medicine);

摘要(Abstract):

目的建立柱后衍生阳离子交换色谱方法,测定鲜竹沥液氨基酸的含量。方法样品加6 mol·L~(-1)盐酸于110℃水解22 h。采用柱后衍生阳离子交换色谱法,对鲜竹沥液氨基酸的含量进行分析。色谱柱:LCAK06/Na型磺酸基强酸性阳离子交换树脂色谱柱(4.6 mm×150 mm,5μm),梯度洗脱,其中A泵(溶液泵)流速为0.45 mL·min~(-1),M泵(茚三酮泵)流速为0.25 mL·min~(-1),检测波长为570 nm,进样量为50μL。结果该测定方法中天冬氨酸、苏氨酸、丝氨酸、谷氨酸、甘氨酸、丙氨酸、缬氨酸、异亮氨酸、亮氨酸、酪氨酸、组氨酸、赖氨酸的线性关系良好,精密度RSD范围为0.67%~1.80%,重复性RSD范围为0.37%~1.79%,平均回收率(n=6)在88.83%~97.99%之间,RSD范围为0.81%~2.88%之间。样品中所含总氨基酸的范围为2.58~1 050.62μg·mL~(-1)。结论所建立的分析方法可作为鲜竹沥液中氨基酸的定量分析。
OBJECTIVE To establish a method for detection of amino acids in Fresh Bamboo Sap.METHODS The sample was hydrolyzed with 6 mol·L~(-1) hydrochloric acid for 22 hours at 110 ℃.The content of amino acids in Fresh Bamboo Sap were detected by cation-exchange chromatography with post-column derivatization.The cation exchange resin LCAK06/Na column(4.6 mm × 150 mm,5 μm) with gradient elution was adopted,where A pump(solution pump) and M pump(ninhydrin pump) were at a flow rate of 0.45 mL·min~(-1) and 0.25 mL·min~(-1),respectively.The detection wavelength was set at 570 nm,and injection volume was 50 μL.RESULTS The method showed a good linear relationship for the determination of aspartate acid,threonine,serine,glutamic acid,proline,glycine,alanine,cystine,valine,methionine,isoleucine,leucine,tyrosine,phenylalanine,histidine,lysine and arginine.The RSD of precision were in the range of 0.67% to 1.8%,the RSD of repeatability were in the range of 0.37% to 1.79%,the average recoveries and RSD were between(n=6),88.83% to 97.99% and 0.81% to 2.88%,respectively.The contents of amino acids ranged from 2.58 to 1 050.62 μg·mL~(-1) in the samples.CONCLUSION The developed method can be applied to the analysis of amino acids in Fresh Bamboo Sap.

关键词(KeyWords): 鲜竹沥;氨基酸;柱后衍生;阳离子交换色谱法
Fresh Bamboo Sap;amino acids;post-column derivatization;cation exchange chromatography

Abstract:

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基金项目(Foundation): 江西省重点研发计划项目(20171BBG70103);; 国家药典委员会药品标准修订(2019Z085)

作者(Author): 洪挺;赵雯;周志强;罗跃华;付辉政;
HONG Ting;ZHAO Wen;ZHOU Zhiqiang;LUO Yuehua;FU Huizheng;Jiangxi Provicial Institute for Drug and Food Control,Jiangxi Provincial Engineering Research Center for Drug and Medical Device Quality,NMPA Key Laboratory for Quality Evaluation of Traditional Chinese Medicine (Traditional Chinese Patent Medicine);

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