摘要
建立了上清液直接进样-高效液相色谱-串联质谱同时测定废水中18种酚类污染物的分析方法。取5.0 mL水样置于具塞离心管中,加氨水调节pH≥12,摇匀,加入1.0 mL二氯甲烷-正己烷(2∶1,v/v)混合溶液并振摇5min,4 000 r/min离心5 min,用玻璃针筒抽取上清液并经0.22μm聚四氟乙烯滤膜过滤,用甲酸调节水样pH至中性;然后采用Thermo Hypersil ODS柱(100 mm×2.1 mm,5.0μm)分离,以甲醇-0.01 mol/L甲酸铵-甲酸水溶液(pH 4.0)为流动相进行梯度洗脱,流速0.2 mL/min,柱温30℃,进样10μL,电喷雾负离子电离(ESI-)模式、多反应监测(MRM)模式进行检测,外标法定量。18种酚类化合物的峰面积与其质量浓度在一定浓度范围内均呈良好的线性关系(r^2≥0.999 1),方法检出限为0.10~0.88μg/L。测定低、中、高加标浓度的样品,18种酚类化合物的相对标准偏差为2.5%~9.9%(n=6);火工药剂废水与石油化工废水样品中的平均加标回收率为68.7%~118%(n=3)。此方法操作简单,灵敏度高,干扰小,分析速度快,可适用于环境废水中18种酚类污染物的同时分析。
A method was developed for the simultaneous determination of 18 phenol pollutants in waste water by high performance liquid chromatography-tandem mass spectrometry（HPLCMS/MS）. A volume of 5. 0 mL waste water was placed into a centrifuge tube. Ammonia was added to the waste water to adjust pH ≥12. A volume of 1. 0 mL methylene chloride-hexane solution（2 ∶1,v/v）was added to the waste water,then the centrifuge tube was oscillated for 5min and centrifuged for 5 min at 4 000 r/min. The water sample was filtered through a 0. 22 μm polytetrafluoroethylene（PTFE） microfiltration membrane and adjusted to neutral by formic acid. With methanol-0. 01 mol/L ammonium formate/formic acid aqueous solution（pH 4. 0）as mobile phase,the separation was performed on a Thermo Hypersil ODS column（100 mm×2. 1mm,5. 0 μm）in gradient elution. The flow rate was 0. 2 mL/min. The column temperature was 30 ℃. The samples were detected by multiple reaction monitoring（MRM）mode with negative electrospray ionization. The phenol pollutants were quantified by external standard method. The calibration curves of the phenol pollutants showed good linearities in a suitable range with correlation coefficients（r-2）not less than 0. 999 1. The detection limits of phenol pollutants ranged from 0. 10 μg/L to 0. 88 μg/L. The relative standard deviations of phenol pollutants were 2. 5%-9. 9%（n = 6）. The average recoveries of the 18 phenol pollutants spiked in waste water samples ranged from 68. 7% to 118%（n = 3）. The method has been proven to be sensitive,rapid and little interference. It is suitable for the determination of the 18 phenol pollutants simultaneously in environmental waste water.
出处
《色谱》
CAS
CSCD
北大核心
2016年第5期473-480,共8页
Chinese Journal of Chromatography
基金
国家环境保护标准制定项目(2014-35)~~
关键词
高效液相色谱-串联质谱法
酚类污染物
废水
high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）
phenol pollutants
waste water
