建立了离子液体超声辅助萃取/液相色谱-质谱联用测定环境水中痕量五氯酚(PCP)的方法。采用离子液体1-丁基-3-甲基咪唑六氟磷酸盐[C4mim][PF6]为萃取剂,考察了试样体积、p H值、温度、超声萃取时间和无机盐含量等因素对PCP萃取效率的影响,试样在XDB C18(150 mm×2.1 mm,5μm)色谱柱上,以甲醇-2 mmol/L醋酸铵溶液(70∶30)为流动相,电喷雾(ESI)电离负离子选择离子监测模式(SIM)进行测定。在优化的萃取条件下,PCP在0.005-1.0μg·L^-1范围内具有良好线性,相关系数(r)为0.999 2,回收率为91.0%-97.0%,日内相对标准偏差(RSD)为1.1%-5.4%,日间RSD为3.8%-8.3%,定量下限为0.005μg·L^-1。建立的方法简便、干扰少、特异性强,可用于环境水样中痕量PCP的测定。
A method was developed for the determination of pentachlorophenol( PCP) in environmental water by liquid chromatography- mass spectrometry( LC- MS) coupled with ultrasonic assisted extraction with ionic liquid. An ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate([C4mim][PF6]),was used as extraction solvent to extract PCP in water samples. The extraction parameters,such as sample volume,temperature,ultrasonic extraction time,inorganic salt concentration and solution p H value were investigated. The chromatographic separation was performed on a XDB C18(150 mm × 2. 1 mm,5 μm) column with a mobile phase of methanol- 2 mmol/L ammonium acetate solution(70 ∶ 30). Detection was carried out by LC- MS using a negative electrospray ionization interface under the selected ion monitoring( SIM) mode. The calibration curve was linear within the range of 0. 005- 1. 0 μg·L- 1with a correlation coefficient of 0. 999 2. The limit of quantitation( LOQ) was 0. 005 μg · L- 1. The extraction recoveries were between 91. 0% and 97. 0%,and the intra-day RSDs were between 1. 1% and 5. 4%,and the inter-day RSDs were between 3. 8%and 8. 3%. The developed method was simple,accurate and specific,and could be used for the determination of trace PCP in environmental water.