高效液相色谱法测定土壤中2,4-二羟基苯甲酸含量  被引量:1

Determination of 2,4-dihydroxy Benzoic Acid Concentration of Soil Using HPLC Method

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作  者:和春庭 张育梅 及利 杨立学[2] 

机构地区:[1]云南省怒江傈僳族自治州林业局,怒江673100 [2]东北林业大学林学院,哈尔滨150040

出  处:《森林工程》2016年第6期34-37,共4页Forest Engineering

基  金:中央高校基本科研业务费专项资金(2572016EAJ1);国家自然科学基金(31170583)

摘  要:建立高效液相色谱法(HPLC)测定土壤中2,4-二羟基苯甲酸含量,分析4种不同土地利用方式土壤中2,4-二羟基苯甲酸的垂直分布趋势.通过用乙酸乙酯水浴24h提取2,4-二羟基苯甲酸,蒸干并溶解于色谱级甲醇中.以流动相为3%冰醋酸和甲醇(75:25)对样品进行洗脱,流速1mL/min,色谱柱为AgilentZORBAX SB-C18(4.6mm×150mm,5μm),检测波长280mn,柱温25尤.结果表明:2,4-二羟基苯甲酸进样浓度在范围内与峰面积呈良好的线性关系,线性回归方程为F=13.315Z-12.803(r2=0.9999);2,4-二羟基苯甲酸的重复性、精密度和稳定性,相对标准偏差(RSD)结果分别为0.778%、1.623%和1.918%,平均加样回收率为97.675%,RSD结果为0.771%(n=6),均达到定性和定量分析的要求.应用高效液相色谱法测定2,4-二羟基苯甲酸含量操作简便、快速、准确,天然次生林土壤中的2,4-二羟基苯甲酸含量大于其余3种土地利用方式的,且4种土地利用方式皆表现出随着土层深度的增加,2,4-二羟基苯甲酸含量降低的趋势.The concentration of 2, 4 - dihydroxy benzoic acid was determined based on the established High Performance Liquid Chromatography (HPLC) method and the amount of 2, 4 - dihydroxy benzoic acid was analyzed in 4 different land uses in the vertical distribution. The 2,4- dihydroxy benzoic acid in sample was extracted by 24 hours - water - bath heating with ethyl acetate, and then was evaporated and dissolved in chromatographic grade methanol. The sample elution was taken by the mobile phase which was composed of 3% glacial acetic acid and methanol (75: 25) with the flowing rate of 1 mL/min. The chromatographic column was Agi-lent ZORBAX SB - C18(4. 6 mm× 150 mm, 5μm) while the detecting wavelength was 280 nm and the column temperature was 25℃. The result showed that a good linear relationship existed between the concentration of 2, 4 - dihydroxy benzoic acid and the peak area in the range of 80 -800 μg/mL. The obtained linear regression equation was F = 13. 315X -12. 803 ( r^2 =0. 999 9) The relative standard deviation (RSD) of repeatability, precision and stability of 2, 4 - dihydroxy benzoic acid were 0. 778% , 1. 623% and 1. 918% respectively. The average recovery rate was 97. 675% and the RSD was 0. 771% ( n =6) , all of which met the requirements of qualitative and quantitative analysis. The determination of 2, 4 - dihydroxy benzoic acid content using HPLC method was simple, rapid and accurate. The amount of the 2,4- dihydroxy benzoic acid in soil of natural secondary forest was found the greatest among 4 kinds of land. A uses and the concentration of 2, 4 - dihydroxy benzoic acid decreased with the depth of the soil.

关 键 词:高效液相色谱法 2 4-二羟基苯甲酸 土地利用方式 

分 类 号:TS47[农业科学—烟草工业] O657.72[理学—分析化学]

 

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