正交试验优化-顶空固相微萃取-气相色谱-串联质谱法测定水中戊二醛

Determination of glutaraldehyde in water by gas chromatography-tandem mass spectrometry with orthogonal test optimization of headspace solid phase microextraction

建立了顶空固相微萃取-气相色谱-串联质谱测定水中戊二醛的方法。设计5因素4水平完整的正交试验,通过极差分析获得顶空固相微萃取优化条件。10 mL,pH 1的水样加入6 g NaCl,经非极性PDM S,100μm纤维头于75℃萃取25 min,210℃解析进样0.2 min。采用VF-5(60 m×0.25 mm×0.25μm)色谱柱程序升温分离,选择多反应监测(M RM)模式采集质谱信息。以m/z 82/54为定量离子,以m/z 82/39为定性离子,外标法定量。结果表明,戊二醛质量浓度在0.02~0.6 mg/L范围内线性良好,相关系数(r)>0.9996,方法检出限7μg/L,定量限20μg/L。低(0.04 mg/L)、中(0.1 mg/L)、高(0.4 mg/L)3个水平加标回收率为87.4%~103.7%,相对标准偏差(RSD)<6%。方法适用于测定水中的戊二醛。

A new method was established to detect glutaraldehyde in water by using headspace solid phase microextraction-chromatography-tandem mass spectrometry.A complete orthogonal test with 5 factors and 4 levels was designed and then the range analysis was used to deal with the experimental data.The optimal headspace solid phase microextraction(HS-SPME)conditions were achieved with 100μm-PDMS fiber,extraction temperature of 75℃,extraction time of 25 min,pH of 1 and NaCl’s weight of 6 g.The desorption was performed for 0.2 min at 210℃.In this study,10 m L water sample was adopted,chromatographic column VF-5(60 m×0.25 mm×0.25μm)was used to proceed temperature programming,and multi reaction monitoring(MRM)was selected to detect the quantitative ion(m/z 82/54)and qualitative ion(m/z 82/39).The quantitation was carried out by the external standard method.The results showed the range of standard curve was 0.02-0.6 mg/L with correlation coefficient(r)>0.9996.In this method,the limit of detection(LOD)was0.007 mg/L,and the limit of quantification(LOQ)was 0.02 mg/L.Moreover,the recoveries of standard and precision experiment were also included in this work according to low(0.04 mg/L),medium(0.1 mg/L)and high(0.4 mg/L)concentration of samples.The recoveries were 87.4%-103.7%with relative standard deviations(RSDs)lower than 6%.This method is suitable for detection of glutaraldehyde in water.