农业环境科学学报2024,Vol.43Issue(9) :2183-2190.DOI:10.11654/jaes.2024-0638

固相萃取净化/GC-MS法测定水/土样品中α-松油醇含量

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

吴凤 区嘉铖 李彦文 赵海明 蔡全英 向垒 莫测辉
农业环境科学学报2024,Vol.43Issue(9) :2183-2190.DOI:10.11654/jaes.2024-0638

固相萃取净化/GC-MS法测定水/土样品中α-松油醇含量

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

吴凤 1区嘉铖 1李彦文 1赵海明 1蔡全英 1向垒 1莫测辉1
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作者信息

  • 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
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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1mL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(R2≥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).

Abstract

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(R2≥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

Key words

organic flotation chemical/beneficiation wastewater/soil/α-terpineol/gas chromatography/mass spectrometry(GC-MS)

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出版年

2024
农业环境科学学报
农业部环境保护科研监测所 中国农业生态环境保护协会

农业环境科学学报

CSTPCD北大核心
影响因子:1.52
ISSN:1672-2043
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