HPLC Determination of D-Serine
摘 要
提出了毋需柱前衍生化处理的高效液相色谱直接测定D型丝氨酸含量的方法。以pH 1.0的高氯酸溶液为流动相,流量为0.3 mL·min-1,Daicel CROWNPAK CR(+)色谱柱(4 mm×150 mm)进行分离,柱温0 ℃。采用170U紫外检测器,检测波长为200 nm,D-丝氨酸及其主要杂质L-丝氨酸在10 min内完全分离,分离度为2.09,其中D-丝氨酸的质量浓度在1.00~10.00 g·L-1范围内呈线性。方法的检出限(3S/N)为0.20 g·L-1,回收率在93.4%~95.7%之间,相对标准偏差(n=6)在3.2%~3.6%之间。
Abstract
A direct method of HPLC without precolumn derivatization was proposed for determination of D-serine. Chromatographic column of Daicel CROWNPAK CR(+) (4 mm×150 mm) and mobile phase of pH 1.0 HClO4 solution were used in the separation, with column temperature of 0 ℃ and flow-rate of 0.3 mL·min-1. 170U UV-detector with wavelength of 200 nm was adopted in the detection. Under the given conditions, the D-serine and its main impurity L-serine were completely separated from each other within 10 min. The resolution factor (Rs) attained to a value of 2.09. Linearity of D-serine was found in the range from 1.00 to 10.00 g·L-1. Detection limit (3S/N) found for the method was 0.20 g·L-1. Tests for recovery and precision were made by standard addition method, values of recovery and RSD′s (n=6) obtained were in the ranges of 93.4%-95.7% and 3.2%-3.6% respectively.
中图分类号 O652.63
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收稿日期 2010/8/18
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备注于荣华(1961-),男,江苏南京人,高级工程师,主要从事海因类化合物等项目的开发及产业化工作。
引用该论文: YU Rong-hua,TAN Jiao-ying,QIAO Hao,LIU Cun-li,YU Wen-tao,WEI Ping. HPLC Determination of D-Serine[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2011, 47(10): 1184~1185
于荣华,谭娇颖,乔浩,刘存礼,于文涛,韦萍. 高效液相色谱法测定D型丝氨酸的含量[J]. 理化检验-化学分册, 2011, 47(10): 1184~1185
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参考文献
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【3】卢昕,刘承伟,卢洁,等.HPLC测定帕金森模型小鼠脑中D-丝氨酸的含量[J].广西师范大学学报, 2009,27(2):68-71.
【4】HASHMOTO K, FUKUSHMA T, SHMIZU E, et al. Possible role of D-serine in pathophysiology of Alzheimer′s disease[J]. Progress in Neuro-Psychopharmacology & Biological Psychiatry, 2004,28:385-388.
【5】HASHMOTO K, ENGBERG G, SHMIZU E, et al. Reduced D-serine to total serine ratio in the cerebrospinal fluid drug nalve schizophrenic patients[J]. Progress in Neuro-Psycho-pharmacology & Biological Psychiatry, 2005,29:767-769.
【6】孙进,吴梧桐,吴震,等.SHMT酶促反应液中L-丝氨酸分离和有关组分分析[J].中国生化药物杂志, 2000,21(3):124-126.
【7】曹飞,荀志金,姚冰,等.甘氨酸铜法制备DL-丝氨酸的研究[J].精细化工, 2001,18(4):232-233.
【8】孙进,吴梧桐,吴震,等.酶法合成L-丝氨酸及反应液中氨基酸的分离[J].中国药科大学报, 2000,31(2):135-138.
【9】成都科学技术大学分析化学教研室.分析化学手册[M].北京:化学工业出版社, 1984.
【10】傅莉,刘信洪,徐春燕,等.HPLC法监测DL-丝氨酸的合成研究[J].北京化工大学学报, 2003,30(4):105-108.
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