液/液萃取-气相色谱/三重四极杆质谱联用法测定水中24种半挥发性有机物

Determination Method of 24 SVOCs in Water by LLE-GC/Triple Quadrupole Mass Spectrometry

建立了液/液萃取-气相色谱/三重四极杆质谱联用法(GC/MS/MS)测定水中24种半挥发性有机物的方法。采用二氯甲烷萃取、多反应监测(MRM)扫描、氘代同位素混合内标定量;0.1~2.0 mg/L质量浓度范围内线性响应良好(响应因子RF的RSD (相对标准偏差)<20%);检出限0.16~0.49μg/L,测定下限0.64~1.96μg/L;RSD范围9.44%~17.2%;目标化合物加标回收率范围73.1%~103.7%,替代物加标回收率范围78.7%~96.8%;该方法抗干扰性强、灵敏度高、定性定量准确,较适用于饮用水源、地表水、地下水、工业废水等环境水体中SVOCs检测。

The determination method of 24 SVOCs in water is established by liquid-liquid extraction(LLE) coupled with gas chromatography/triple quadrupole mass spectrometry(GC/MS/MS). Sample was extracted by dichloromethane, scanned under MRM mode and quantified with deuterium isotope mixed internal standard. the linear relationship between peak area and concentration was good enough(response factor RSD < 20%) from 0.1 to 2.0 mg/L. The method detection limit was 0.16 ~ 0.49 μg/L and the method quantification limit was 0.64 ~ 1.96 μg/L. RSD was 9.44%~ 17.2%. The recovery rate of the target compounds was 73.1%~ 103.7%, and that of the surrogate standard was 78.7%~ 96.8%. The result shows that the proposed method is strong anti-interference,highly sensitive and highly efficient. The method is suitable for the determi-nation of 24 SVOCs in source water, surface water, underground water, industrial wastewater and so on.