通过对色谱条件和样品前处理方法进行优化,建立固相萃取—亲水作用色谱法测定香菇(Lentinula edodes)中硫杂脯氨酸的检测方法。优化后的色谱条件为:Inertsil HILIC亲水作用色谱柱(4.6×250 mm,5μm)对样品进行分离测定,流动相采用乙腈-0.1%磷酸水(85∶15,v/v)等度洗脱,流速0.8mL/min,检测波长193nm,柱温30℃。前处理方法为:香菇样品采用甲醇-水(70∶30,v/v)提取,MAX阴离子固相萃取小柱进行净化处理,甲醇-1.0%甲酸(90∶10,v/v)作为洗脱剂对目标物进行洗脱。检测结果表明,硫杂脯氨酸在2~100μg/mL范围内呈良好的线性关系,相关系数为0.9998,加标回收率为96.3%~101.7%,相对标准偏差在1.3%~4.8%之间,检出限为0.76μg/g,定量限为2.31μg/g。该方法回收率高、简单、快速、无需衍生化,适用于香菇子实体硫杂脯氨酸的定量检测分析。 Through the optimization of chromatographic conditions and sample pretreatment methods, the determination of thia-proline in Lentinula edodes by solid-phase extraction-hydrophilic interaction chromatography was established. The optimized chromatographic conditions were as follows: the Inertsil HILIC hydrophilic interaction column (4.6 × 250 mm, 5μm) was used to separate the sample and the mobile phase was isocratic eluted with acetonitrile-0.1% phosphoric acid water (85:15, v / v) , Flow rate 0.8mL / min, detection wavelength 193nm, column temperature 30 ℃. The pretreatment methods were as follows: the mushroom samples were extracted with methanol-water (70:30, v / v), MAX anion SPE cartridges were eluted with methanol-methanol 1.0% formic acid (90:10, v / v) The target is eluted. The results showed that thiophene proline showed a good linearity in the range of 2 ~ 100μg / mL, the correlation coefficient was 0.9998, the recoveries were 96.3% ~ 101.7%, and the relative standard deviations were between 1.3% ~ 4.8% , The detection limit was 0.76μg / g, the limit of quantification was 2.31μg / g. The method has the advantages of high recovery rate, simple and rapid, without derivatization, and is suitable for the quantitative detection and analysis of the thymol-proline in fruiting bodies of mushrooms.