CAJ | 학술논문

研究了整体柱离子对色谱结合紫外检测的方法分析对甲苯磺酸根( C7 H7 SO3-)。采用反相硅胶整体柱,以氢氧化四丁基铵-柠檬酸-乙腈为流动相,考察了紫外检测波长、流动相组成、色谱柱温度和流速对离子保留的影响。色谱条件经过优化,在紫外检测波长230 nm,流动相为0．4 mmol·L-1氢氧化四丁基胺( TBA)-0．13 mmol·L-1柠檬酸-15%(v/v)乙腈(pH 5．5),流速3．0 mL·min-1,柱温40℃的条件下,C7H7SO3-的保留时间为1．25 min内。常见无机阴离子( Cl-,NO3-)不干扰测定。在0．7~100 mg·L-1范围内,线性回归方程的相关系数为0．9997,峰面积的相对标准偏差(RSD,n=5)为1．0%,检出限(S/N=3)为0．2 mg·L-1。该方法应用于检测实验室合成离子液体中的C7 H7 SO3-,加标回收率为101%。方法简单、快速。
연구료정체주리자대색보결합자외검측적방법분석대갑분광산근( C7 H7 SO3-)。채용반상규효정체주,이경양화사정기안-저몽산-을정위류동상,고찰료자외검측파장、류동상조성、색보주온도화류속대리자보류적영향。색보조건경과우화,재자외검측파장230 nm,류동상위0．4 mmol·L-1경양화사정기알( TBA)-0．13 mmol·L-1저몽산-15%(v/v)을정(pH 5．5),류속3．0 mL·min-1,주온40℃적조건하,C7H7SO3-적보류시간위1．25 min내。상견무궤음리자( Cl-,NO3-)불간우측정。재0．7~100 mg·L-1범위내,선성회귀방정적상관계수위0．9997,봉면적적상대표준편차(RSD,n=5)위1．0%,검출한(S/N=3)위0．2 mg·L-1。해방법응용우검측실험실합성리자액체중적C7 H7 SO3-,가표회수솔위101%。방법간단、쾌속。
In this article,ion-pair chromatography with ultraviolet detection was used in the analysis of p-toluenesulfonate. The ana-lyte was separated using a mobile phase of tetrabutylammonium hydroxide( TBA)-citric acid-acetonitrile on a reversed-phase silica-based monolithic column. The ultraviolet detection wavelength,the composition of mobile phase,column temperature and flow rate on the ion retention and separation were investigated,retention rule was discussed. The chromatographic conditions were optimized:at 230 nm wavelength,when 0. 4 mmol·L-1 TBA-0. 13 mmol·L-1 citric acid-15%(v/v)acetonitrile(pH 5. 5)was used as mobile phase with column temperature of 40℃ and flow rate of 3. 0 mL·min-1 ,retention time of C7 H7 SO3-was less than 1. 25 min. Common inor-ganic anions( Cl-,NO3-) did not interfere with the determination. In the range of 0. 7-100 mg·L-1 ,the correlation coefficient of line-ar regression equation was 0. 9997. Relative standard deviation(RSD)of chromatographic peak area was 1. 0%(n=5). Detection limit(S/N=3)was 0. 2 mg·L-1. The method has been applied to the determination of p-toluenesulfonate ionic liquid samples syn-thesized by chemistry laboratory. Standard addition recovery rate was 101%. The method was simple and rapid.