高效液相色谱-串联质谱法同时测定水体和沉积物中12种有机磷酸酯类化合物

发布时间：2018-06-22 09:24

  本文选题：有机磷酸酯 + 高效液相色谱-串联质谱法　； 参考：《分析化学》2017年07期

【摘要】：建立了高效液相色谱-质谱联用技术结合固相萃取和液液萃取方法检测水体和沉积物中12种磷酸酯类(OPEs)化合物残留的方法。水样样品经HLB固相萃取柱富集,乙酸乙酯洗脱两次,沉积物样品以乙腈超声萃取,旋转蒸发至干,用超纯水稀释后重复水样处理步骤,采用ZORBAX Eclipse Plus C_(18)色谱柱(150 mm×2.1 mm,3.5μm)进行分离,以0.2%甲酸-甲醇作为流动相进行梯度洗脱,采用正离子MRM监测模式,外标法定量分析。水样中,12种OPEs在0.05、0.10和0.50μg/L加标水平下,除TMP(28.5%~47.8%)和TEHP(22.4%~73.8%)外,其余目标化合物的平均回收率为66.4%~115.0%,相对标准偏差为0.5%~9.1%,方法定量限(MOQ)为0.001~0.050μg/L;沉积物中,在5、10和50μg/kg加标水平下,除TMP(35.7%~44.9%)、TCEP(31.2%~48.9%)外,其余目标化合物的平均回收率为65.9%~120.0%,相对标准偏差为0.01%~9.5%,方法定量限(MOQ)为0.02~2.0μg/kg(dw)。基于上述方法对太湖水样和沉积物样品中目标化合物定量检测分析,∑OPEs含量分别为0.1~1.7μg/L和8.1~420μg/kg dw。
[Abstract]:A high performance liquid chromatography-mass spectrometry (HPLC-MS) method combined with solid phase extraction (SPE) and liquid-liquid extraction (LLE) was developed for the determination of 12 phosphate compounds residues in water and sediment. The water sample was enriched by HLB solid phase extraction column and eluted twice by ethyl acetate. The sediment sample was extracted by acetonitrile ultrasonic extraction, rotated evaporated to dry, then diluted with ultrapure water and repeated the water sample treatment step. The sample was separated by ZORBAX Eclipse Plus C _ (18) column (150mm 脳 2.1 mm ~ 3.5 渭 m). Gradient elution was carried out with 0.2% formic acid-methanol as mobile phase. Positive ion MRM monitoring mode and external standard method were used for quantitative analysis. The average recoveries of 12 kinds of OPEs in water samples were 66.4% and 115.0%, with the exception of TMP (28.57.8%) and TEHP (22.43.8%) at 0.05 渭 g / L and 0.50 渭 g / L, respectively. The relative standard deviation was 0.59.1%, and the quantitative limit (MOQ) was 0.001 ~ 0.050 渭 g / L; in sediments, at the addition level of 5n10 and 50 渭 g/kg, TCEP (35.744.9%) was increased to 48.9%. The average recoveries of the remaining target compounds were 65.9% and 120.0, the relative standard deviation was 0.01 and 9.5.The quantitative limit (MOQ) of the method was 0.02 渭 g/kg (dw). Based on the above method, the contents of 鈭，

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