CAJ | 학술논문

建立了高效液相色谱串联质谱技术(Liquid chromatography tandem mass spectrometry, LC- MS/ MS)同时测定土壤中邻苯二甲酸酯(Phthalic acid esters, PAEs)的分析方法。确定了土壤样品加速溶剂萃取最优条件是以正己烷为萃取溶剂,在160℃下,静态萃取4次,每次12 min,萃取液经旋转蒸发浓缩,以乙腈-0.1%甲酸溶液为流动相梯度洗脱分离后,用 LC-MS/ MS 结合大气压化学源(Atmospheric pressure chemical ionization, APCI)进行定性及定量分析。土壤中11种 PAEs 的浓度与其峰面积呈良好的线性关系,检出限为0.03~13.0μg/ kg,样品的加标平均回收率为72.8%~101.8%,相对标准偏差(RSD)为1.7%~6.7%。方法简便快速,且灵敏度高,适用于土壤中11种邻苯二甲酸酯的同时测定。
건립료고효액상색보천련질보기술(Liquid chromatography tandem mass spectrometry, LC- MS/ MS)동시측정토양중린분이갑산지(Phthalic acid esters, PAEs)적분석방법。학정료토양양품가속용제췌취최우조건시이정기완위췌취용제,재160℃하,정태췌취4차,매차12 min,췌취액경선전증발농축,이을정-0.1%갑산용액위류동상제도세탈분리후,용 LC-MS/ MS 결합대기압화학원(Atmospheric pressure chemical ionization, APCI)진행정성급정량분석。토양중11충 PAEs 적농도여기봉면적정량호적선성관계,검출한위0.03~13.0μg/ kg,양품적가표평균회수솔위72.8%~101.8%,상대표준편차(RSD)위1.7%~6.7%。방법간편쾌속,차령민도고,괄용우토양중11충린분이갑산지적동시측정。
A sensitive and convenient method based on accelerated solvent extraction ( ASE )-liquid chromatography tandem mass spectrometry (LC-MS / MS) was established for the simultaneous determination of 11 phthalic acid esters(PAEs) in soil. The optimized conditions were as follows: By using n-hexane as the extraction solvent, spiked sample was extracted by ASE at 160 ℃ for 4 times, 12 min for each time. The extract was concentrated by evaporation. Qualitative and quantitative analysis was carried out by the multiple reaction monitoring mode after the chromatographic separation with atmospheric pressure chemical ionization (APCI), using acetonitrile -0. 1% formic acid water as mobile phase. The limits of detection(LODs) for 11 PAEs were between 0. 03 - 13. 0 μg / kg. The recoveries and relative standard deviations were 72. 8% -101. 8% and 1. 7-6. 7% , respectively. This method is rapid, sensitive and suitable for the determination of PAEs in soil.