高效液相色谱法检测土壤中二硫化二苯并噻唑

Detection of MBTS in soil by high performance liquid chromatography

目的建立土壤中二硫化二苯并噻唑(MBTS)检测的高效液相色谱法。方法通过乙腈超声萃取30 min,有机滤膜过滤器过滤,且通过C18柱净化,使用HPLC分析仪器,设定流速0.7 mL/min;柱温40℃,在检测波长275 nm对土样进行分离定性及外标法定量。结果对MBTS检测前处理和色谱条件优化得到,乙腈作为萃取溶剂,C18柱作为净化柱。适当的梯度洗脱程序,对降低土壤中基质效应对分析目标化合物有较好的作用。进行方法学验证得出,MBTS加标精密度相对标准偏差范围在0.070%~0.201%之间,MBTS加标正确度相对标准偏差范围在0.071%~0.646%之间,加标回收率范围在91.0%~97.1%。MBTS方法检出限为0.003 mg/kg,测定下限为0.013 mg/kg。结论该方法具有操作简单,检出限低,测试时间短,干扰小,精密度和准确度高等优点,可以为土壤中MBTS的检测提供技术支撑。

Objective To establish a high-performance liquid chromatography method for the detection of dibenzothiazole disulfide(MBTS)in soil.Methods Extract using acetonitrile ultrasound for 30 minutes,filter through an organic membrane filter,and purify through a C18 column.Use an HPLC analyzer with set flow rate of 0.7 mL/min and column temperature of 40℃,and the soil sample is separated for qualitative analysis and quantitative analysis using external standard method at a detection wavelength of 275 nm.Results By optimizing the pre-treatment and chromatographic conditions for MBTS detection,acetonitrile was used as the extraction solvent,C18 column serves as the purification column.An appropriate gradient elution program has a good effect on reducing matrix effects in soil and analyzing target compounds.Through methodological validation,it was found that,the relative standard deviation of MBTS spiked precision ranges from 0.070%to 0.201%.The relative standard deviation of MBTS spiking accuracy ranges from 0.071%to 0.646%,and the spiking recovery rate ranges from 91.0%to 97.1%,the detection limit of MBTS method is 0.003 mg/kg,and the lower limit of determination is 0.013 mg/kg.Conclusion This method has the advantages of simple operation,low detection limit,short testing time,low interference,high precision and accuracy,and can provide technical support for the MBTS in soil.