CAJ | 학술논문

建立了固相萃取-超高效液相色谱-电喷雾串联三重四极杆质谱联用技术分析水中16种全氟有机化合物的高通量检测方法。样品经 WAX 固相萃取柱富集和净化后，采用 Waters ACQUITY UPLCTM BEH C18色谱柱，含2 mmol/L乙酸铵的甲醇和含2 mmol/L乙酸铵的水作为流动相进行梯度洗脱，质谱采用电喷雾负离子电离，多反应监测模式检测。16种全氟有机化合物在0.5~100μg/L或1.0~100μg/L 浓度范围内线性关系良好，相关系数为0.9987~0.9999，方法的检出限为0.06~0.46 ng/L；高、中、低3个添加水平的回收率为67.6％~103％，相对标准偏差为2.94％~12.0％。结果表明，该方法灵敏、准确且检测范围广，分析速度快，是一种适于实际水样中全氟有机化合物检测分析的方法。
건립료고상췌취-초고효액상색보-전분무천련삼중사겁간질보련용기술분석수중16충전불유궤화합물적고통량검측방법。양품경 WAX 고상췌취주부집화정화후，채용 Waters ACQUITY UPLCTM BEH C18색보주，함2 mmol/L을산안적갑순화함2 mmol/L을산안적수작위류동상진행제도세탈，질보채용전분무부리자전리，다반응감측모식검측。16충전불유궤화합물재0.5~100μg/L혹1.0~100μg/L 농도범위내선성관계량호，상관계수위0.9987~0.9999，방법적검출한위0.06~0.46 ng/L；고、중、저3개첨가수평적회수솔위67.6％~103％，상대표준편차위2.94％~12.0％。결과표명，해방법령민、준학차검측범위엄，분석속도쾌，시일충괄우실제수양중전불유궤화합물검측분석적방법。
A high-throughput detection method has been developed for the determination of six-teen perfluorinated organic compounds( PFCs)in surface water by solid phase extraction-ultra performance liquid chromatography coupled with electrospray ionization tandem mass spec-trometry( SPE-UPLC-ESI-MS/MS). The water samples were concentrated and purified through WAX solid phase extraction cartridges. The UPLC separation was performed on an ACQUITY UPLCTM BEH C18 column utilizing a gradient elution program of methanol(containing 2 mmol/L ammonium acetate)and water( containing 2 mmol/L ammonium acetate)as the mobile phases at a flow rate of 0. 4 mL/min. The MS/MS detection was performed under negative electrospray ionization( ESI-)in multiple reaction monitoring( MRM)mode. Good linearities were observed in the range of 0. 5-100 μg/L or 1. 0-100 μg/L with correlation coefficients from 0. 998 7 to 0. 999 9. The limits of detection( LODs)for the sixteen perfluorinated organic compounds were in the range of 0. 06-0. 46 ng/L. The recoveries ranged from 67. 6% to 103% with the relative standard deviations between 2. 94% and 12. 0%. This method was characterized by high sensitiv-ity and precision,extensive range and high speed,and can be applied for the analysis of PFC contaminants in surface water.