藏药牦牛血粉饮片中氨基酸和无机元素测定

Determination of amino acids and inorganic elements in Tibetan medicine yak blood powder decoction pieces

为建立藏药牦牛血粉饮片中氨基酸和无机元素的定性和定量分析方法,试验采用高效液相色谱-柱后衍生法对牦牛血粉中游离氨基酸进行测定:离子交换柱(2.5 mm×150 mm,6μm),检测波长为570 nm、440 nm,测试方法为单点矫正法;采用微波消解-ICP-MS对牦牛血粉中无机元素进行测定:测定模式为碰撞反应模式,碰撞气(He)流量5 mL/min。数据采集模式:跳峰扫描,采样深度8.0 mm,重复扫描3次。结果表明:牦牛血粉中含有一定量的游离氨基酸,其中包括8种人体必须氨基酸。无机元素以Al、Na、Mg、K、Ca、Fe为主,还含有V、Cr、Mn、Zn、Co、Ni、Cu、Se等人体所需微量元素,各无机元素均在浓度考察范围内,线性关系良好(r^2>0.9984),加样回收率在99.2%~108.4%之间。该研究初步明确藏药牦牛血粉饮片中氨基酸和无机元素的组成,方法准确高效,为综合评价藏药牦牛血粉饮片的质量提供科学依据和方法参考。

In order to establish a qualitative and quantitative analysis method of amino acids and inorganic elements in Tibetan medicine yak blood powder decoction pieces,the free amino acids were determined by high performance liquid chromatography with post-column derivatization.Chromatographic analysis was achieved using a ion exchange column(2.5 mm×150 mm,6μm).The detection wavelength was 570 nm and 440 nm and the test method was single point correction method.The inorganic elements were determined by ICP-MS after microwave digestion.The determination mode was collision reaction mode,and the flow rate of collision gas(He)was 5 mL/min.Data acquisition mode was skip peak scanning,the sampling depth was 8.0 mm and scanning 3 times.The results showed that yak blood powder decoction pieces contained a certain amount of free amino acids,including eight essential amino acids.The inorganic elements were mainly Al,Na,Mg,K,Ca and Fe.They also contained trace elements such as V,Cr,Mn,Zn,Co,Ni,Cu,Se and so on.All the inorganic elements showed good linearity(r^2>0.9984).The average recovery was 99.2%-108.4%.In this paper,the composition of amino acids and inorganic elements in Tibetan yak blood powder decoction pieces was preliminarily clarified.This method is accurate and efficient,which can be used for scientific basis and method reference for the comprehensive evaluation of Tibetan Medicine Yak Blood powder decoction pieces.