土壤2023，Vol.60Issue(5)：1152-1159,8.DOI:10.13758/j.cnki.tr.2023.05.027
高效液相色谱分析土壤氨基糖的质量控制方法
Quality Control for Determining Amino Sugar Contents in Soil by High Performance Liquid Chromatography
摘要
Abstract
Four amino sugars,namely,muramic acid(MurN),mannosamine(ManN),galactosamine(GalN)and glucosamine(GluN),in soil were determined by ortho-phthalaldehyde(OPA)pre-column derivatisation-high performance liquid chromatography(HPLC).The sensitivity,precision and accuracy of the instrument and method were tested from chromatographic peaks,theoretical plates,signal-noise(S/N)ratio,limits of detection and quantification,sample content repeatability,standard linearity,and recovery.The results showed that the chromatographic peak orders of the four amino sugars were MurN,ManN,GalN and GluN.The chromatographic peak shapes were good and the resolutions of each two adjacent peaks were>1.5,indicating that the two adjacent peaks were completely separated.Theoretical plates were>2 000,indicating high chromatographic column efficiency.The instrument detection limits of MurN,ManN,GalN and GluN were 0.030,0.300,0.150 and 0.150 μmol/L,the instrument quantitative limits were 0.100,1.000,0.500 and 0.500 μmol/L,the method detection limits were 0.010,1.500,0.100 and 0.100 μmol/L,and the method quantitative limits were 0.030,5.000,0.300 and 0.300 μmol/L,respectively.In addition to ManN in the soil below 10 cm,S/N ratios of the amino sugars amount were all>10,indicating high sensitivity of the instrument and method.The relative standard deviations of the amino sugar amount in the parallel standard samples,parallel soil samples and repeated soil samples were all<5%,indicating high precision of the instrument and method.The R2 values of the standard curve were>0.997 0,and the recovery rates of blank and soil substrate were between 80%and 94%,indicating high accuracy of the instrument and method.In conclusion,the method for the determination of soil amino sugar content by OPA pre-column derivatisation-HPLC,which is simple in operation and high in sensitivity,could accurately determine the contents of amino sugar in soils.关键词
OPA柱前在线衍生/微生物残体/灵敏度/精密度/准确度Key words
OPA pre-column derivatisation/Microbial necromass/Sensitivity/Precision/Accuracy分类
农业科技引用本文复制引用
杨洋,张心昱,张应华,于颖超,董欣妮..高效液相色谱分析土壤氨基糖的质量控制方法[J].土壤,2023,60(5):1152-1159,8.基金项目
国家自然科学基金项目(31170435)和内蒙古自治区研究生教育创新计划项目(S20210202Z)资助Supported by the National Natural Science Foundation of China(No.31170435)and the Graduate Education Innovation Program of Inner Mongolia Autonomous Region of China(No.S20210202Z) （31170435）
