色谱
色譜
색보
Chinese Journal of Chromatography
2015年
9期
988-994
,共7页
徐中其%叶峰%王永乐%李爱梅
徐中其%葉峰%王永樂%李愛梅
서중기%협봉%왕영악%리애매
压力辅助电动进样%毛细管电泳%西酞普兰%高灵敏度手性拆分
壓力輔助電動進樣%毛細管電泳%西酞普蘭%高靈敏度手性拆分
압력보조전동진양%모세관전영%서태보란%고령민도수성탁분
pressure-assisted electrokinetic injection ( PAEKI)%capillary electrophoresis ( CE)%citalopram%highly sensitive enantioseparation
应用压力辅助电动进样( pressure?assisted electrokinetic injection, PAEKI)技术开发了毛细管电泳( CE)对阳离子手性药物西酞普兰( citalopram, CIT)拆分的高灵敏度分析方法。在电动进样( electrokinetic injection, EKI)过程中,由于CIT的两个对映异构体与手性选择试剂( sulfated?β?cyclodextrin, S?β?CD)之间的动态平衡常数存在差异而导致了电动歧视效应。因此,在EKI过程前向毛细管中充满不含手性选择剂的背景电解质,从而抑制电动进样歧视。通过两个步骤优化PAEKI过程中的关键参数得到电渗流和反向压力之间的平衡条件。在最优的PAEKI条件下(+10 kV,0?2 psi(约1?4 kPa)),两个对映异构体在205 nm紫外检测条件下的检出限( LOD;S/N=3)达到1?1和2?2 ng/mL。灵敏度较常规的压力进样平均提高了62倍,方法的检测灵敏度达到了ng/mL ( ppb),有望成为检测人体体液中CIT对映异构体的有效方法。
應用壓力輔助電動進樣( pressure?assisted electrokinetic injection, PAEKI)技術開髮瞭毛細管電泳( CE)對暘離子手性藥物西酞普蘭( citalopram, CIT)拆分的高靈敏度分析方法。在電動進樣( electrokinetic injection, EKI)過程中,由于CIT的兩箇對映異構體與手性選擇試劑( sulfated?β?cyclodextrin, S?β?CD)之間的動態平衡常數存在差異而導緻瞭電動歧視效應。因此,在EKI過程前嚮毛細管中充滿不含手性選擇劑的揹景電解質,從而抑製電動進樣歧視。通過兩箇步驟優化PAEKI過程中的關鍵參數得到電滲流和反嚮壓力之間的平衡條件。在最優的PAEKI條件下(+10 kV,0?2 psi(約1?4 kPa)),兩箇對映異構體在205 nm紫外檢測條件下的檢齣限( LOD;S/N=3)達到1?1和2?2 ng/mL。靈敏度較常規的壓力進樣平均提高瞭62倍,方法的檢測靈敏度達到瞭ng/mL ( ppb),有望成為檢測人體體液中CIT對映異構體的有效方法。
응용압력보조전동진양( pressure?assisted electrokinetic injection, PAEKI)기술개발료모세관전영( CE)대양리자수성약물서태보란( citalopram, CIT)탁분적고령민도분석방법。재전동진양( electrokinetic injection, EKI)과정중,유우CIT적량개대영이구체여수성선택시제( sulfated?β?cyclodextrin, S?β?CD)지간적동태평형상수존재차이이도치료전동기시효응。인차,재EKI과정전향모세관중충만불함수성선택제적배경전해질,종이억제전동진양기시。통과량개보취우화PAEKI과정중적관건삼수득도전삼류화반향압력지간적평형조건。재최우적PAEKI조건하(+10 kV,0?2 psi(약1?4 kPa)),량개대영이구체재205 nm자외검측조건하적검출한( LOD;S/N=3)체도1?1화2?2 ng/mL。령민도교상규적압력진양평균제고료62배,방법적검측령민도체도료ng/mL ( ppb),유망성위검측인체체액중CIT대영이구체적유효방법。
Pressure?assisted electrokinetic injection ( PAEKI) was applied to the highly sensitive enantiosepara?tion of the positively charged drug citalopram ( CIT) by capillary electrophoresis ( CE) . It was found that the in?jection discrimination occurred in electrokinetic injection ( EKI) process due to the different dynamic equilibri?um constant between chiral selector ( sulfated?β?cyclodextrin, S?β?CD) and two isomers of CIT. Herein, it was proposed to use the background electrolyte ( BGE) without chiral selector to fill the capillary, and then start the EKI step to eliminate the injection discrimination of free analytes. The critical parameters in PAEKI could be optimized in two steps to seek the balance between the electroosmotic flow ( EOF ) and the counterbalance pressure. Under the optimized PAEKI conditions (+10 kV, 0?2 psi ( ca. 1?4 kPa) ) , the obtained LODs ( S/N=3) of the two isomers were 1?1 and 2?2 ng/mL under UV detection ( 205 nm) , which was averaged 62?fold im?proved in comparison with normal hydrodynamic injection ( HDI) . The proposal offered ng/mL ( ppb) level sen?sitivity of CIT determination and could be an effective method in the applications in human body biofluids.