摘要
开发了弱阴离子交换柱固相萃取+高效液相色谱-负电喷雾-串联质联法[WAX-SPE+HPLC-ESI(-)-MS/MS]检测污水中碳链长度在2-14内的全氟羧酸(PFCAs).采用弱阴离子交换(WAX)柱进行固相萃取时,将污水水样用甲酸酸化至pH=3.0,并使用2%甲酸溶液作净化溶剂、1%氢氧化铵甲醇溶液作洗脱溶剂,则可使短长链PFCAs(C2-C14)均具有较高的回收率,并克服了反相固相萃取柱对短链PFCAs(C2-C5)回收率低的缺点.为了验证方法的有效性,对上海市市政污水处理厂A和B的进水进行检测,结果表明各种PFCAs的回收率分别在56%-121%和54%-120%的范围内,相对标准偏差(RSD)分别小于11%和14%,方法检出限和定量限分别在0.2-1.0 ng/L和1.0-5.0 ng/L的范围内,这充分证明了该方法的可靠性.此外,在处理厂A和B内含量最高的PFCAs均为全氟辛酸(分别为743 ng/L和837 ng/L),其次为三氟乙酸(分别为139 ng/L和489 ng/L).
A method using weak anion exchange cartridge for solid phase extraction before high performance liquid chromatography-negative electronspray ionization-tandem mass spectrometry [WAX-SPE + HPLC-ESI(-)-MS/MS] detection has been developed to measure C2-C14 perfluorocarboxylates (PFCAs) in sewages. When the weak anion exchange (WAX) cartridges were used for solid phase extraction (SPE), the better recoveries of short- and long-chain PFCAs (C2-C 14) were achieved as the sewage samples were acidified to pH = 3.0 by formic acid, 2% formic acid was used for washing solvent and 1% ammonium hydroxide in methanol was used for elution solvent. The WAX cartridges used for SPE overcame the disadvantages of reverse phase solid phase extraction cartridges, i.e. the recoveries of short-chain PFCAs (C2-C5) were very low. The validity of this method was demonstrated by determination of short- and long-chain PFCAs (C2-C14) in influent of municipal wastewater treatment plant A and B in Shanghai, China. The results indicate that the recoveries of all PFCAs in influent of plant A and B are 56%-121% and 54%-120%, respectively; the recovery relative standard deviations (RSD) of plant A and B are 〈 11% and 〈 14%, respectively; and the method detection limits (MDL) and method quantitation limits (MQL) are 0. 2-1.0 ng/L and 1.0-5.0 ng/L, respectively. In addition, the perfluorooctanoate (743 ng/L and 837 ng/L, respectively) and trifluoroacetic acid (139 ng/L and 489 ng/L, respectively) are the most and the second most PFCAs found in both plant A and B.
出处
《环境科学》
EI
CAS
CSCD
北大核心
2009年第9期2647-2654,共8页
Environmental Science
基金
国家自然科学基金项目(20807032)
江苏省环境科学与工程省重点实验室开放课题项目(ZD061203)
污染控制与资源化国家重点实验室开放课题项目(PCRRF06007)
长江水环境教育部重点实验室开放课题项目(YRWEF07002)
关键词
全氟羧酸
弱阴离子交换柱
固相萃取
高效液相色谱-串联质谱仪
污水
perfiuorocarboxylates (PFCAs)
weak anion exchange cartridge
solid phase extraction (SPE)
high performance liquid chromatography-tandem mass spectrometry
sewages