离子液体超声辅助萃取/LC-MS法测定环境水中痕量五氯酚  

Determination of Pentachlorophenol in Environmental Water by LC- MS and Ultrasonic Assisted Extraction with Ionic Liquid

作　　者：闵剑青[1] 陈梅兰[1] 陈晓红[2,3] 金米聪[2,3] 

机构地区：[1]浙江树人大学生物与环境工程学院,浙江杭州310015 [2]宁波市疾病预防控制中心浙江省微量有毒化学物健康风险评估技术研究重点实验室,浙江宁波315010 [3]宁波市疾病预防控制中心宁波市毒物研究与控制重点实验室,浙江宁波315010

出　　处：《分析测试学报》2015年第4期438-442,共5页Journal of Instrumental Analysis

基　　金：国家自然科学基金项目(20977083;21377114);浙江省自然科学基金项目(LY14B070004;LZ14B070001)

摘　　要：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.

关 键 词：超声辅助萃取 液-液微萃取 离子液体 水 五氯酚 液相色谱-质谱联用法 

分 类 号：O657.63[理学—分析化学] O625.32[理学—化学]