摘要
发展了丙酸和丁酸的反相色谱-间接紫外检测分析方法。用反相硅胶整体柱,以对氨基苯酚盐酸盐-有机溶剂为流动相分离测定丙酸和丁酸。研究了对氨基苯酚盐酸盐和有机溶剂对分离和测定的影响,探讨了保留规律。结果表明,在柱温30℃,流速2.0 m L·min^(-1),以0.7 mmol·L^(-1)对氨基苯酚盐酸盐水溶液(pH 4.5)-甲醇(v∶v=90∶10)为流动相条件下,丙酸和丁酸在3 min之内完全分离,检出限分别为0.12和0.21 mg·L^(-1)。将方法应用于白酒的测定,加标回收率在98.6%~98.8%之间,相对标准偏差小于1.1%。本方法快速、准确、可靠。
An analytical method was developed for the determination of propionic acid and butyric acid by reversed-phase liquidchromatography with indirect ultraviolet detection. Chromatographic separation of propionic acid and butyric acid was performed on areversed-phase silica-based monolithic column using 4-aminophenol hydrochloride aqueous solution-organic solvent as mobilephase. The effects of the organic solvents and 4-aminophenol hydrochloride on the separation and determination of propionic acidand butyric acid were investigated. The retention rules of the propionic acid and butyric acid under different chromatographic conditionswere discussed. The successful separation of propionic acid and butyric acid was obtained using 0. 7 mmol·L-1 4-aminophenolhydrochloride aqueous solution(pH 4. 5) methanol(v ∶v =90 ∶10)as mobile phase at the column temperature of 30 oC and the flowrate of 2. 0 mL·min-1 . Under the optimal conditions,the baseline separations of propionic acid and butyric acid were successfully achievedin 3. 0 min. The detection limits(S / N =3)for propionic acid and butyric acid were 0. 12 and 0. 21 mg·L-1 ,respectively.The method has been successfully applied to the determination of two aliphatic acids in white spirit sample. Recoveries of the aliphaticacids after spiking were 98. 6% -98. 8%. This method is rapid,accurate and reliable.
作者
张小东
卜文
刘峰
于泓
卜文
刘峰
于泓
ZHANG Xiao-dong;BU Wen;LIU Feng;YU Hong(College of Chemistry and Chemical Engineering,Harbin Normal University,Harbin 150025,China;Qiqihar Mineral Exploration and Development General Institute of Heilongjiang Province,Qiqihar 161006,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2016年第7期1020-1024,共5页
Chemical Research and Application
基金
黑龙江省自然科学基金项目(B201307)资助
关键词
反相色谱
间接紫外检测
丙酸
丁酸
对氨基苯酚盐酸盐
reversed-phase liquid chromatography
indirect ultraviolet detection
propionic acid
butyric acid
4-aminophenol hydrochloride
