QuEChERS-HPLC法测定土壤中麦角甾醇含量  

A new QuEChERS-HPLC method for determining ergosterol in soil

作　　者：曹梦 李勇[1,2,3] 孙忠祥[1,2,3] 兴安 冯晓晓[4] 黄元仿 张红艳 CAO Meng;LI Yong;SUN Zhong-xiang;XING An;FENG Xiao-xiao;HUANG Yuan-fang;ZHANG Hong-yan(College of Resources and Environmental Sciences,China Agricultural University,Beijing 100193;Key Laboratory of Arable Land Conservation in North China,the Ministry of Agriculture,Beijing 100193;Key Laboratory of Land Quality,Ministry of Land andResources,Beijing 100193;College of Science,China Agricultural University,Beijing 100193)

机构地区：[1]中国农业大学资源与环境学院,北京100193 [2]农业部华北耕地保育重点实验室,北京100193 [3]国土资源部农用地质量与监控重点实验室,北京100035 [4]中国农业大学理学院,北京100193

出　　处：《分析试验室》2019年第2期162-166,共5页Chinese Journal of Analysis Laboratory

基　　金：国家重点研发计划项目(2016YFD0300801)资助

摘　　要：结合QuEChERS法与高效液相色谱(HPLC)技术,建立了一种土壤中麦角甾醇的快速检测方法。以甲醇为提取溶剂,N-丙基-乙二胺(PSA)为吸附剂,实现了样品的快速提取净化;利用Agilent HC-C18色谱柱(250 mm×4. 6 mm,5μm)进行HPLC分离,以甲醇为流动相,紫外检测器于280 nm波长处检测,基质匹配标准溶液外标法定量。结果表明,麦角甾醇在0. 01～10. 00 mg/L浓度范围内具有良好的线性关系(R^2> 0. 999);在添加浓度为0. 5,1. 0和5. 0 mg/kg的添加回收试验中,平均回收率为87. 6%～92. 8%,相对标准偏差(RSD)为0. 82%～3. 0%,方法的定量限为0. 5 mg/kg。该方法可以直接用于土壤样品中麦角甾醇的含量检测,并已成功分析了山西省安太堡露天煤矿的28个土样。A rapid,simple and reliable QuEChERS method was modified,developed and validated for the determination of ergosterol in soil samples combined with high-performance hquid chromatograph (HPLC).After extraction with methanol and purification enrichment,the extract was purified by primary second amine (PSA).An Agilent HC-C18 column (250 mm×4.6 ram,5μm)was employed for the separation of the ergosterol and other nontarget compounds.The mobile phase was methanol at a flow rate of 1.0 mL/min and the detection wavelength was 280 nm.Quantitative analysis of ergosterol in soil was validated by the external standard method using the matched standard solution to compensate for matrix effect.This method showed good linearity in the concentrations between 0.01 and 10.00 mg/L with the coefficient of determination (R^2 )value >0.999.The average recoveries were 87.6%-92.8 %spiked at the levels of 0.5,1.0 and 5.0 mg/kg with relative standard deviations (RSDs)of 0.82 %-3.0 %,and the limit quantification of this method was 0.5 mg/kg.With the advantages of operation and accuracy,this proposed method has been successfully applied to the analysis of 28 soil samples obtained from Antaibao opencast mine,Shanxi Province,China.

关 键 词：QUECHERS 高效液相色谱 土壤 麦角甾醇 

分 类 号：S132[农业科学—农业基础科学]