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    超高效液相色谱-串联质谱法快速测定地表水中5种污染物

    Rapid Determination of 5 Pollutants in Surface Water by UHPLC-MS/MS

    • 摘要: 地表水样品采集于棕色玻璃瓶中,经0.2 μm聚醚砜针式滤头过滤,采用超高效液相色谱-串联质谱法快速测定滤液中苯胺、联苯胺、微囊藻毒素-LR、甲萘威、丙烯酰胺等5种污染物的含量。以ACQUITY UPLC®BEH C8色谱柱为固定相,以不同体积比的甲醇和0.1%(体积分数)甲酸溶液的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾离子源正离子模式和多反应监测模式。5种污染物的质量浓度在一定范围内与其对应的质谱响应强度呈线性关系,检出限为0.04~0.10 μg·L-1。以空白地表水样品为基体进行加标回收试验,所得回收率为95.0%~120%,测定值的相对标准偏差(n=6)为1.9%~12%。

       

      Abstract: The surface water sample was collected in a brown glass bottle, and then filtered on 0.2 μm polyethersulfone needle filter. UHPLC-MS/MS was applied to the rapid determination of 5 pollutants, i.e. aniline,benzidine, microcystin-LR, carbaryl and acrylamide in the filtrate. ACQUITY UPLC®BEH C8 chromatographic column was used as stationary phase, and the mixture of methanol and 0.1% (volume fraction) formic acid solution mixed in different ratios was used as mobile phase in gradient elution. ESI+ and multi-reactions monitor mode were adopted in MS/MS. Linear relationships between values of intensity of mass spectral response and mass concentration of the 5 pollutants were kept in definite ranges, with detection limits in the range of 0.04-0.10 μg·L-1. On the base of blank surface water sample, test for recovery was made by standard addition method; values of recovery found were in the range of 95.0%-120%, with RSDs (n=6) of determined values in the range of 1.9%-12%.

       

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