色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
6期
629-634
,共6页
丁怡然%黄云%赵婷婷%蔡倩%罗玉%黄斌%张榆霞%潘学军
丁怡然%黃雲%趙婷婷%蔡倩%囉玉%黃斌%張榆霞%潘學軍
정이연%황운%조정정%채천%라옥%황빈%장유하%반학군
衍生化%固相萃取%气相色谱-质谱法%有机紫外防晒剂%水样
衍生化%固相萃取%氣相色譜-質譜法%有機紫外防曬劑%水樣
연생화%고상췌취%기상색보-질보법%유궤자외방쇄제%수양
derivatization%solid phase extraction ( SPE )%gas chromatography-mass spectrometry(GC-MS)%organic ultraviolet filters%water sample
建立了水体中5种典型有机紫外防晒剂甲氧基肉桂酸乙基己酯(ethylhexyl methoxycinnamate,EHMC)、二苯酮-3(benzophenone-3,BP-3)、4-甲基苄亚基樟脑(4-methylbenzylidene camphor,4-MBC)、奥克立林( octo-crylene,OC)和胡莫柳酯(homosalate,HMS)的气相色谱-质谱检测方法。对 HMS、BP-3衍生化条件进行了系统的优化。以100μL 双(三甲基硅烷基)三氟乙酰胺( N,O-bis( trimethylsilyl)trifluoroacetamide,BSTFA)为衍生化试剂,在100℃下反应100 min。水样固相萃取选用 Oasis HLB 萃取柱(0.5 g),洗脱溶剂为乙酸乙酯-二氯甲烷(1∶1,v / v),水样 pH 3~5。该方法对5种化合物的检出限范围为0.5~1.2 ng / L,定量限范围为1.4~4.0 ng / L。最佳实验条件下,加标水样回收率为87.85%~102.34%,相对标准偏差(n =3)均小于5%。该方法成功地应用于昆明市第一污水厂进出口水样中目标物质的分析。
建立瞭水體中5種典型有機紫外防曬劑甲氧基肉桂痠乙基己酯(ethylhexyl methoxycinnamate,EHMC)、二苯酮-3(benzophenone-3,BP-3)、4-甲基芐亞基樟腦(4-methylbenzylidene camphor,4-MBC)、奧剋立林( octo-crylene,OC)和鬍莫柳酯(homosalate,HMS)的氣相色譜-質譜檢測方法。對 HMS、BP-3衍生化條件進行瞭繫統的優化。以100μL 雙(三甲基硅烷基)三氟乙酰胺( N,O-bis( trimethylsilyl)trifluoroacetamide,BSTFA)為衍生化試劑,在100℃下反應100 min。水樣固相萃取選用 Oasis HLB 萃取柱(0.5 g),洗脫溶劑為乙痠乙酯-二氯甲烷(1∶1,v / v),水樣 pH 3~5。該方法對5種化閤物的檢齣限範圍為0.5~1.2 ng / L,定量限範圍為1.4~4.0 ng / L。最佳實驗條件下,加標水樣迴收率為87.85%~102.34%,相對標準偏差(n =3)均小于5%。該方法成功地應用于昆明市第一汙水廠進齣口水樣中目標物質的分析。
건립료수체중5충전형유궤자외방쇄제갑양기육계산을기기지(ethylhexyl methoxycinnamate,EHMC)、이분동-3(benzophenone-3,BP-3)、4-갑기변아기장뇌(4-methylbenzylidene camphor,4-MBC)、오극립림( octo-crylene,OC)화호막류지(homosalate,HMS)적기상색보-질보검측방법。대 HMS、BP-3연생화조건진행료계통적우화。이100μL 쌍(삼갑기규완기)삼불을선알( N,O-bis( trimethylsilyl)trifluoroacetamide,BSTFA)위연생화시제,재100℃하반응100 min。수양고상췌취선용 Oasis HLB 췌취주(0.5 g),세탈용제위을산을지-이록갑완(1∶1,v / v),수양 pH 3~5。해방법대5충화합물적검출한범위위0.5~1.2 ng / L,정량한범위위1.4~4.0 ng / L。최가실험조건하,가표수양회수솔위87.85%~102.34%,상대표준편차(n =3)균소우5%。해방법성공지응용우곤명시제일오수엄진출구수양중목표물질적분석。
A method for the determination of five representative organic UV filters:ethylhexyl methoxycinnamate ( EHMC ), benzophenone-3 ( BP-3 ), 4-methylbenzylidene camphor ( 4-MBC),octocrylene( OC),homosalate( HMS)in water was investigated. The method was based on derivatization,solid phase extraction( SPE ),followed by determination with gas chromatography-mass spectrometry( GC-MS). The variables involved in the derivatization of BP-3 and HMS were optimized,and SPE conditions were studied. For derivatization,100 μL N,O-bis( trimethylsilyl)trifluoroacetamide( BSTFA)was used as derivatization reagent and reacted with BP-3 and HMS at 100 ℃ for 100 min. For SPE,the pH value of water sample was adjusted to 3-5. The Oasis HLB cartridges were employed and the solution of ethyl acetate and dichloromethane(1 ∶1,v / v)was used as the eluting solvent,and good recoveries of the target compounds were obtained. The limits of detection( LODs) and the limits of quantification (LOQs)for the five target compounds in water samples were 0. 5-1. 2 ng / L and 1. 4-4. 0 ng / L, respectively. The recoveries of spiked water samples were 87. 85% -102. 34% with good repeat-ability and reproducibility(RSD﹤5% ,n = 3)for all the target compounds. Finally,the validated method was applied to analysis the representative UV filters in water samples collected from a wastewater treatment plant in Kunming city of Yunnan province.