CAJ | 학술논문

采用高效液相色谱-同位素稀释串联质谱法( LC-ID-MS/MS)建立了土壤和蚯蚓中手性α-,β-,γ-六溴环十二烷( HBCD)的分离分析方法。样品添加d18-HBCDs作为同位素内标后提取,土壤样品采用正己烷-二氯甲烷(1：1, V/V)作萃取剂,加速溶剂萃取(ASE),硅胶固相萃取小柱净化；蚯蚓样品采用乙酸乙酯涡旋超声提取,浓硫酸磺化后过硅胶小柱净化。α-,β-,γ-HBCD各对映体的线性范围为0.25~50 ng/mL；土壤中检出限为0.00544~0.00766 ng/g,定量限为0.0173~0.0244 ng/g,在0.05和2.5 ng/g添加浓度的回收率为80.0％~95.9％,相对标准偏差RSD为5.7％~11.9％；在蚯蚓中,检出限为0.0103~0.0148 ng/g,定量限为0.0328~0.0471 ng/g,在0.1和5.0 ng/g添加浓度的回收率为78.0％~94.4％,相对标准偏差RSD为6.1％~12.2％。可满足实际样品的测定要求。
채용고효액상색보-동위소희석천련질보법( LC-ID-MS/MS)건립료토양화구인중수성α-,β-,γ-륙추배십이완( HBCD)적분리분석방법。양품첨가d18-HBCDs작위동위소내표후제취,토양양품채용정기완-이록갑완(1：1, V/V)작췌취제,가속용제췌취(ASE),규효고상췌취소주정화；구인양품채용을산을지와선초성제취,농류산광화후과규효소주정화。α-,β-,γ-HBCD각대영체적선성범위위0.25~50 ng/mL；토양중검출한위0.00544~0.00766 ng/g,정량한위0.0173~0.0244 ng/g,재0.05화2.5 ng/g첨가농도적회수솔위80.0％~95.9％,상대표준편차RSD위5.7％~11.9％；재구인중,검출한위0.0103~0.0148 ng/g,정량한위0.0328~0.0471 ng/g,재0.1화5.0 ng/g첨가농도적회수솔위78.0％~94.4％,상대표준편차RSD위6.1％~12.2％。가만족실제양품적측정요구。
An enantioselective method was developed for the separation and determination of three chiral hexabromocyclododecanes ( HBCDs ) including α-HBCD, β-HBCD, γ-HBCD in soil and earthworm by HPLC-ID-MS/MS. d18-HBCDs used as internal standards were added to the samples before extraction. HBCDs enantiomers were extracted from soil by accelerated solvent extraction ( ASE ) with n-hexane/DCM (1:1,V/V) at 100℃ and 10 MPa for 5 min, and further cleaned up using silica column. HBCDs enantiomers were extracted from earthworm by vortex turbulence with ethyl acetate. The extracts were orderly sulphonated by sulfuric acid, and purified by silica column. For all HBCDs enantiomers, good linearities were obtained in the concentration range of 0. 25-50 ng/mL. Limits of detection ( LOD) and limits of quantification ( LOQ) were 0. 00544-0. 00766 ng/g and 0. 0173-0. 0244 ng/g, respectively in soil. The recoveries of spiked samples at 0. 05 and 2. 5 ng/g levels were 80. 0%-95. 9% with relative standard deviations ( RSD, %) of 5. 7%-11. 9% in soil. Limits of detection (LOD) and limits of quantification (LOQ) were 0. 0103-0. 0148 ng/g and 0. 0328-0. 0471 ng/g, respectively in earthworm. The recoveries of spiked samples at 0. 1 and 5 ng/g levels were 78. 0% -94. 4% with relative standard deviations ( RSD, %) of 6. 1% -12. 2% in earthworm. This method can meet the requirements of determination of trace HBCDs in soil and earthworm.