CAJ | 학술논문

采用固相萃取-气相色谱-质谱联用技术，建立了水体中9种药品及个人护理用品（水杨酸、萘普生、布洛芬、对乙酰氨基酚、降固醇酸、三氯生、双氯酚酸、酮洛芬和双酚 A）的定量分析方法。水样品经稀盐酸调节至 pH =3后，采用 Oasis HLB 固相萃取小柱进行富集净化；选用三甲基氢氧化硫（ TMSH）为衍生化试剂，在常温条件下对目标物进行快速甲基化；以气相色谱-质谱法选择离子监测模式（GC-MS-SIM）进行检测，由2，4，5-涕丙酸为内标进行定量分析。本实验分别对固相萃取和衍生化等前处理条件进行了系统的研究。在优化的实验条件下，方法的回收率为50.7~115.4％，相对标准偏差均不高于10％，检出限为0.03~0.30μg / L，定量限为0．15~1．50μg / L。利用该方法对东莞市某农田灌溉水进行了分析，4种目标物在样品中有检出，最大质量浓度范围为0.176~0.998μg / L。结果表明该方法操作简便，灵敏可靠。
채용고상췌취-기상색보-질보련용기술，건립료수체중9충약품급개인호리용품（수양산、내보생、포락분、대을선안기분、강고순산、삼록생、쌍록분산、동락분화쌍분 A）적정량분석방법。수양품경희염산조절지 pH =3후，채용 Oasis HLB 고상췌취소주진행부집정화；선용삼갑기경양화류（ TMSH）위연생화시제，재상온조건하대목표물진행쾌속갑기화；이기상색보-질보법선택리자감측모식（GC-MS-SIM）진행검측，유2，4，5-체병산위내표진행정량분석。본실험분별대고상췌취화연생화등전처리조건진행료계통적연구。재우화적실험조건하，방법적회수솔위50.7~115.4％，상대표준편차균불고우10％，검출한위0.03~0.30μg / L，정량한위0．15~1．50μg / L。이용해방법대동완시모농전관개수진행료분석，4충목표물재양품중유검출，최대질량농도범위위0.176~0.998μg / L。결과표명해방법조작간편，령민가고。
An analytical method has been developed and validated for the simultaneous deter-mination of nine pharmaceuticals and personal care products(PPCPs)in water samples,inclu-ding salicylic acid,naproxen,ibuprofen,paracetamol,clofibric acid,triclosan,diclofenac, ketoprofen,bisphenol A. The qualification and quantification of the target compounds were per-formed by gas chromatography-mass spectrometry in selected ion monitoring mode( GC-MS-SIM). The water samples were concentrated and purified through Oasis HLB cartridges after the pH value of the water was adjusted to 3,then derivatized with trimethyl sulfonium hydroxide (TMSH)at room temperature,and determined by GC-MS-SIM using 2,4,5-fenoprop as internal standard. The conditions for sample pretreatment( e. g. solid phase extraction and derivatiza-tion)were studied. Under the optimized conditions,the recoveries were ranged from 50. 7% to 115. 4% with the relative standard deviations lower than 10% . The limits of detection were in the range of 0. 03-0. 30 μg / L and the limits of quantification were in the range of 0.15-1.50 μg / L. The method has been successfully applied to monitor the occurrence of the PPCPs residues in agricultural irrigation water in Dongguan,Guangdong Province. The four compounds were detected at maximum mass concentration range of 0. 176-0. 998 μg / L. It proved that this analyt-ical method is sensitive,reliable and acceptable.