超高效液相色谱—质谱法快速测定工作场所空气中光气

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

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0.5~150μg/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0.1μg/mL,最低检出浓度为3.3×10-4mg/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。

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 C18column 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.