色谱
色譜
색보
Chinese Journal of Chromatography
2015年
10期
1065-1070
,共6页
毛细管内固相萃取法%气相色谱%烷基酚%辛基酚%壬基酚%纺织品
毛細管內固相萃取法%氣相色譜%烷基酚%辛基酚%壬基酚%紡織品
모세관내고상췌취법%기상색보%완기분%신기분%임기분%방직품
in-tube capillary solid-phase extraction(SPE)%gas chromatography(GC)%alkyl phenols(APs)%octylphenol%nonylphenol%textile
建立了毛细管内固相萃取（ SPE）-气相色谱（ GC）检测纺织品中壬基酚和辛基酚含量的分析方法。通过比较4种性质不同固相萃取剂的萃取效果，筛选出对烷基酚（ APs）类物质萃取效果最佳的固相萃取剂，将其作为填充物质制作毛细管内固相萃取柱，将毛细管内固相萃取法与气相色谱联用进行分析检测。最佳固相萃取剂为 Abselut NEXUS，毛细管内固相萃取最佳条件为：1.2μL 甲醇和1.2μL 超纯水活化，1.2μL 甲醇洗脱，上样速率是0.4μL／min。该法在较低浓度范围内呈现良好的线性相关性，对烷基酚的富集倍数约为100倍，对辛基酚和壬基酚的检出限分别为3.7μg／L和4.5μg／L，加标回收率分别为85.6％~98.2％和83.8％~95.7％，结果表明，此法能够简捷、迅速、有效地检测出纺织品中残留的烷基酚类物质。
建立瞭毛細管內固相萃取（ SPE）-氣相色譜（ GC）檢測紡織品中壬基酚和辛基酚含量的分析方法。通過比較4種性質不同固相萃取劑的萃取效果，篩選齣對烷基酚（ APs）類物質萃取效果最佳的固相萃取劑，將其作為填充物質製作毛細管內固相萃取柱，將毛細管內固相萃取法與氣相色譜聯用進行分析檢測。最佳固相萃取劑為 Abselut NEXUS，毛細管內固相萃取最佳條件為：1.2μL 甲醇和1.2μL 超純水活化，1.2μL 甲醇洗脫，上樣速率是0.4μL／min。該法在較低濃度範圍內呈現良好的線性相關性，對烷基酚的富集倍數約為100倍，對辛基酚和壬基酚的檢齣限分彆為3.7μg／L和4.5μg／L，加標迴收率分彆為85.6％~98.2％和83.8％~95.7％，結果錶明，此法能夠簡捷、迅速、有效地檢測齣紡織品中殘留的烷基酚類物質。
건립료모세관내고상췌취（ SPE）-기상색보（ GC）검측방직품중임기분화신기분함량적분석방법。통과비교4충성질불동고상췌취제적췌취효과，사선출대완기분（ APs）류물질췌취효과최가적고상췌취제，장기작위전충물질제작모세관내고상췌취주，장모세관내고상췌취법여기상색보련용진행분석검측。최가고상췌취제위 Abselut NEXUS，모세관내고상췌취최가조건위：1.2μL 갑순화1.2μL 초순수활화，1.2μL 갑순세탈，상양속솔시0.4μL／min。해법재교저농도범위내정현량호적선성상관성，대완기분적부집배수약위100배，대신기분화임기분적검출한분별위3.7μg／L화4.5μg／L，가표회수솔분별위85.6％~98.2％화83.8％~95.7％，결과표명，차법능구간첩、신속、유효지검측출방직품중잔류적완기분류물질。
An in-tube capillary solid-phase extraction( SPE)-gas chromatography( GC)meth-od was developed for confirmation and quantitative determination of octylphenol ( OP ) and nonylphenol( NP)in textiles. To make the in-tube capillary SPE column,the best SPE car-tridge was chosen from four kinds of SPE cartridges. The adsorbent in the cartridge was used as the filling material to make the in-tube capillary SPE column. The nature,volume used,flow rate and adsorption capacity of the eluent were compared. Finally,the in-tube capillary solid-phase extraction was combined with gas chromatography to detect the alkyl phenols( APs ). Abselut NEXUS extraction cartridge was chosen as the best solid phase extractant. The optimal in-tube capillary SPE extraction conditions were as follows:1. 2 μL methanol and 1. 2 μL ultra-pure water for activating the extraction column,1. 2 μL methanol for eluting,0. 4 μL/min for solution loading. The method showed a good linear relationship in the low concentration range, and the enrichment ratios for the APs were about 100 times. The detection limits of octylphenol and nonylphenol were 3. 7 μg/L and 4. 5 μg/L,respectively. The recoveries of octylphenol were 85. 6%-98. 2%,and those of nonylphenol were 83. 8%-95. 7%. The experimental results demon-strated that the method is simple,rapid,and useful for detecting APs in textiles.
