建立了一种抑制电导检测-离子色谱(IC)同时测定草甘膦生产工艺中母液里的草甘膦及其副产物、无机阴离子的方法.样品经过滤后直接进样,色谱条件:IonPac AS11-HC分离柱(250 mm ×4 mm)和IonPac AG11-HC保护柱(50 mm×4 mm),在线淋洗液发生器KOH梯度淋洗,流速1.0 mL/min,采用抑制电导检测.草甘膦、甲基草甘膦、六甲基磷酰三胺(HMPA)、增甘膦、亚磷酸、磷酸、Cl-和SO42-的线性范围分别为0.1~20 mg/L、0.1~20 mg/L、0.1~50 mg/L、0.25~50 mg/L、0.05~20 mg/L、0.2~50 mg/L、0.02~20 mg/L和0.05~50 mg/L,相关系数分别为0.9995、0.9993、0.9999、0.9998、0.9999、0.9985、0.9999和0.9980,加标回收率为93.7%~104.0%,相对标准偏差均小于2.5%(n=7),检出限(以信噪比(S/N)=3计)为0.002~0.025 mg/L.该方法用于草甘膦生产工艺中母液里草甘膦及其含磷副产物和无机阴离子的测定,结果令人满意.
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