分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2015年
1期
81-86
,共6页
陈新%倪鑫炯%张佳瑜%刘瑛%曹玉华
陳新%倪鑫炯%張佳瑜%劉瑛%曹玉華
진신%예흠형%장가유%류영%조옥화
微乳毛细管电泳%大体积进样%pH动态连接%扫集%多环芳烃( PAHs)
微乳毛細管電泳%大體積進樣%pH動態連接%掃集%多環芳烴( PAHs)
미유모세관전영%대체적진양%pH동태련접%소집%다배방경( PAHs)
Microemulsion electrokinetic chromatography%Large volume sample stacking%Dynamic pH junction%Sweeping%Polycyclic aromatic hydrocarbons
要建立了反向微乳毛细管电泳( MEEKC)在线富集技术灵敏检测多环芳烃的方法。采用大体积进样_pH动态连接_扫集微乳毛细管电泳法( LVSS_DypH_MEEKC)对于常规条件下很难分离的6种强亲脂性的多环芳烃中性分子进行富集分离。结果表明,在反相电压下,当微乳液的组成为:2.4%( w/w) SDS、0.6%(w/w)正辛烷、6.6%(w/w)正丁醇、20 mmol/L NaH2PO4缓冲液(pH 2.2);进HCB时间为20 s(16 kPa),进样时间为80 s(16 kPa)时,富集效果良好,富集倍数在25~80倍之间,在27 min内实现了对多环芳烃化合物的灵敏检测。将本方法用于化妆品中多环芳烃的检测,回收率在90.6%~95.9%之间,相对标准偏差均小于5.1%(n=5)。
要建立瞭反嚮微乳毛細管電泳( MEEKC)在線富集技術靈敏檢測多環芳烴的方法。採用大體積進樣_pH動態連接_掃集微乳毛細管電泳法( LVSS_DypH_MEEKC)對于常規條件下很難分離的6種彊親脂性的多環芳烴中性分子進行富集分離。結果錶明,在反相電壓下,噹微乳液的組成為:2.4%( w/w) SDS、0.6%(w/w)正辛烷、6.6%(w/w)正丁醇、20 mmol/L NaH2PO4緩遲液(pH 2.2);進HCB時間為20 s(16 kPa),進樣時間為80 s(16 kPa)時,富集效果良好,富集倍數在25~80倍之間,在27 min內實現瞭對多環芳烴化閤物的靈敏檢測。將本方法用于化妝品中多環芳烴的檢測,迴收率在90.6%~95.9%之間,相對標準偏差均小于5.1%(n=5)。
요건립료반향미유모세관전영( MEEKC)재선부집기술령민검측다배방경적방법。채용대체적진양_pH동태련접_소집미유모세관전영법( LVSS_DypH_MEEKC)대우상규조건하흔난분리적6충강친지성적다배방경중성분자진행부집분리。결과표명,재반상전압하,당미유액적조성위:2.4%( w/w) SDS、0.6%(w/w)정신완、6.6%(w/w)정정순、20 mmol/L NaH2PO4완충액(pH 2.2);진HCB시간위20 s(16 kPa),진양시간위80 s(16 kPa)시,부집효과량호,부집배수재25~80배지간,재27 min내실현료대다배방경화합물적령민검측。장본방법용우화장품중다배방경적검측,회수솔재90.6%~95.9%지간,상대표준편차균소우5.1%(n=5)。
A sensitive analytical method based on reversed microemulsion electrokinetic chromatography ( MEEKC) combined with on_line preconcentration technique was developed for the determination of polycyclic aromatic hydrocarbons ( PAHs ) in cosmetics. For six lipophilic PAHs analytes which are difficult to be separated under conventional conditions, three stacking techniques including large volume sample stacking ( LVSS) , dynamic pH junction and sweeping ( LVSS_DypH_sweep ) were combined to realize the efficient preconcentration and separation. Under the optimum conditions, including the microemulsion buffer with the composition of 2. 4%(w/w)SDS_0. 6% (w/w) octane_6. 6% (w/w)n_butyl alcohol_20 mmol/L NaH2PO4 ( pH 2 . 2 ) , HCB injection time of 20 s ( 16 kPa ) and sample injection time of 80 s ( 16 kPa ) , good enrichment effect was reached with the enrichment factors ranged from 25 to 80 , and the PAHs were analyzed successfully within 27 min. The developed method was used to analyze the PAHs in cosmetics. The recoveries ranged from 90 . 6% to 95 . 9%. The RSD values ( n=5 ) were less than 5 . 1%.