固相萃取净化/GC-MS法测定水/土样品中α-松油醇含量  

Determination ofα-terpineol in aqueous and soil samples using solid-liquid extraction purification coupled with gas chromatography/mass spectrometry

作　　者：吴凤 区嘉铖 李彦文 赵海明 蔡全英 向垒 莫测辉 WU Feng;OU Jiacheng;LI Yanwen;ZHAO Haiming;CAI Quanying;XIANG Lei;MO Cehui(Guangdong Provincial Research Center for Environment Pollution Control and Remediation Materials,College of Life Science and Technology,Jinan University,Guangzhou 510632,China)

机构地区：[1]暨南大学生命科学技术学院,广东省环境污染控制与修复材料工程中心,广州510632

出　　处：《农业环境科学学报》2024年第9期2183-2190,共8页Journal of Agro-Environment Science

基　　金：国家重点研发计划项目(2020YFC1807600)。

摘　　要：采用固相萃取净化结合GC-MS法分别建立了测定水/土样品中典型有机浮选药剂(α-松油醇)的方法。采用DB-5 MS进行色谱分离,电子轰击(EI)-选择离子检测(SIM)和基质标线进行定量分析。水/土样品均采用二氯甲烷进行萃取,水样萃取时,先将其pH值和盐度调整为7.5和0.5%,之后采用二氯甲烷进行3次萃取;土壤萃取时采用二氯甲烷进行2次振荡萃取,萃取液旋转蒸发近干后用1 mL甲醇定容为萃取质。水、土样品萃取质均采用C18小柱进行固相萃取净化。在上述最优萃取条件下,目标化合物在0.1~5 mg·L^(-1)浓度范围内线性关系良好(R^(2)≥0.998);其在水/土样品中的检出限(LOD)分别为0.027~0.041 mg·L^(-1)(水样)和0.009~0.054 mg·kg^(-1)(土样),在实际样品中不同浓度(1、2、5 mg·L^(-1)或1、2、5 mg·kg^(-1))加标回收率分别为91.5%~112%[相对标准偏差(RSD)<15%,水样]和67%~114%(RSD<15%,土样)。Methods for the determination of typical organic flotation reagent(α-terpineol)in water and soil samples were respectively established using solid phase extraction(SPE)purification and gas chromatography/mass spectrometry(GC-MS).Chromatographic separation of the analyte was performed using DB-5 MS,and its quantitative analysis was performed using electron bombardment(EI)-selected ion monitoring(SIM)and matrix-matched calibrations.Both water and soil samples were extracted with dichloromethane.For water sample,pH and salinity were adjusted to 7.5 and 0.5%,respectively,followed by three times of liquid-liquid extraction using dichloromethane as extractant.For soil sample,dichloromethane was used for oscillatory extraction twice.The extract was evaporated to dryness and then diluted to 1 mL with methanol as the extract.The extracts of water and soil samples were purified by solid phase extraction using a C18 cartridge.Under the optimal extraction conditions described above,the analyte showed a good linear relationship in the concentration range of 0.1~5 mg·L^(-1)(R^(2)≥0.998).Its limit of detection(LOD)was determined as 0.027 mg·L^(-1)to 0.041 mg·L^(-1)(water samples)and 0.009 mg·kg^(-1)to 0.054 mg·kg^(-1)(soil samples),respectively.Its recoveries of spiked samples at different concentrations(1,2,5 mg·L^(-1)or 1,2,5 mg·kg^(-1))were 91.5%to 112%[Relative standard deviation(RSD)<15%,water samples]and 67%to 114%(RSD<15%,soil samples),respectively.

关 键 词：有机选冶药剂 选矿废水 土壤 松油醇 GC-MS 

分 类 号：X830.2[环境科学与工程—环境工程] O657.63[理学—分析化学]