超高效液相色谱-质谱法快速测定工作场所空气中光气

杨华梅; 杭莉

超高效液相色谱-质谱法快速测定工作场所空气中光气

杨华梅,
杭莉

Determination of Phosgene in Air at Workplace by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

摘要

摘要:
目的建立超高效液相色谱-串联三重四极杆质谱(UPLC-ESI-MS/MS)联用技术快速测定工作场所空气中光气的方法。
方法样品经采集后, 目标化物以Waters ACQUITY UPLCTM BEH C₁₈色谱柱为分离柱, 以甲醇和含0.002 mol/L乙酸铵水溶液为流动相进行梯度洗脱, 电喷雾离子源电离、正离子多反应监测模式质谱进行定性和定量分析。
结果目标化合物在0.5~150 μg/L质量浓度范围内线性良好, 相关系数为0.9998, 仪器方法的检出限(以3倍信噪比计)为0.1 μg/mL, 最低检出浓度为3.3×10^-4 mg/m³(以采集7.5 L空气计算); 高、中、低3个添加水平的回收率为88.0%~97.5%, 相对标准偏差为1.30%~3.18%。
结论该方法灵敏、准确, 检测范围广, 分析速度快。

Abstract:
Objectives To develop a method for the determination of phosgene in the air at workplace by ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS).
Methods After air samples being collected, the target compound was separated in an ACQUITY UPLCTM system by BEH C₁₈ column with methanol and water (both containing 0.002 mol/L ammonium acetate) andgradient elution, and was determined qualitatively and quantitatively by electrospray positive ionization (ESI+) and multiple reaction monitoring (MRM).
Results The target compound was in a good linearity between 0.5 and 150 μg/L, the correlation coefficient of calibration curves was 0.9998, the limit of detection (LOD) was 0.1 μg/L (take the signal to noise ration as 3), the minimum detection limit (MDL) was 3.3×10^-3mg/m³(in a sample volume of 7.5 L), the recovery of standard addition at three levels was 88.0%~97.5%, the relative standard deviation (RSD) was less than 5% (n=6).
Conclusions The method is characterized by high sensitivity and precision, extensive analytical range and quickly analytical rate and it can be used for the determination of phosgene in air at workplace.

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