雷丸中16种氨基酸的柱前衍生化RP-HPLC法含量测定  

Pre-column derivatization RP-HPLC determination of 16 amino acids in Omphalia lapidescens Schroet.

作　　者：郑灏 程显隆[2] 魏锋[2] 肖新月[2] 林玉莲 

机构地区：[1]江苏省盐城药品检验所,盐城224002 [2]中国药品生物制品检定所,北京100050

出　　处：《药物分析杂志》2011年第9期1631-1635,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：科技部重大专项“中药质量标准研究和信息化体系建设平台”(2009ZX09308-004)

摘　　要：目的:测定雷丸中16种氨基酸的含量。方法:样品以6 mol.L-1盐酸于150℃水解1 h,以异硫氰酸苯酯(PITC)为衍生化试剂衍生后进行HPLC分析。采用Phenomenex Luna C18(250 mm×4.6 mm,5μm)色谱柱,柱温为43℃;流动相A为0.1mol.L-1醋酸钠缓冲液(以醋酸调pH 6.5)-乙腈(93∶7),流动相B为乙腈-水(4∶1),梯度洗脱,流速为1.0 mL.min-1;检测波长为254 nm。结果:16种氨基酸浓度在1.16～47.32μg.mL-1范围内呈良好的线性关系(r=0.9998～1.000);平均回收率在93.3%～107.2%之间;RSD均小于3.0%。结论:本方法灵敏、准确,具有良好的重复性和稳定性,可用于雷丸中氨基酸的检测。Objective：To determine and analyze 16 amino acids in Omphalia lapidecsens Schroet.Methods：The sample was hydrolyzed for 1 hour at 150 ℃,and derivatized with phenyl isothiocyanate（PITC）.HPLC was performed on a Phenomenex C18（4.6 mm×250 mm,5 μm）column with gradient elution of 0.1 mol·L-1 sodium acetate buffer solution（adjusted to pH 6.5 with acetic acid）-acetonitrile（93∶7）（A）and acetonitrile-water（4∶1）（B）at the flow rate of 1.0 mL·min-1,detected at 254 nm.Column temperature was 43 ℃.Results：16 amino acids had good linearity in the ranges of 1.16-47.32 μg·mL-1（r=0.9998-1.000）.The average recoveries were 93.3%-107.2%,and RSDs were less than 3.0%.Conclusion：The method is sensitive and accurate with good stability,which is useful for the determination of amino acids in Omphalia lapidecsens Schroet.

关 键 词：中药 真菌 菌核 雷丸 衍生化 氨基酸 异硫氰酸苯酯 高效液相色谱 

分 类 号：R917[医药卫生—药物分析学]