高效液相色谱柱后化学发光检测技术对杉科植物中羟基酸的分析应用  

Application of HPLC with post-column chemiluminescence detection to alcoholic acid in Taxodium ascendens and Taxodium distichum

作　　者：高智席[1] 周光明[2] 唐国风[1] 吴永平[1] 

机构地区：[1]遵义师范学院化学系,遵义563002 [2]西南大学化学化工学院,重庆400715

出　　处：《药物分析杂志》2007年第7期1081-1085,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:本文建立了用高效液相色谱分离柱后化学发光法测定杉科植物中羟基酸含量。方法:基于在酸性介质中高锰酸钾直接氧化酒石酸、苹果酸和莽草酸等羟基酸产生化学发光,而盐酸氨基脲能够显著增强该体系的发光强度。采用 kBPCL 超微弱发光测量仪作为检测器,Hypersil ODS(4.6mm×150mm,5μm)柱,高氯酸(pH=2.5)溶液为流动相,流速0.8mL·min^(-1)。结果:酒石酸、苹果酸和莽草酸浓度分别在8.6×10^(-7)～2.6×10^(-4)(r=0.9991),9.6×10^(-8)～3×10^(-4)(r=0.9999),2.2×10^(-7)～3.5×10^(-3)g·mL^(-1)(r=0.9998)范围内,与峰面积有良好的线性关系;检出限分别为3.54×10^(-8),2.24×10^(-9),2.02×10^(-8)g·mL^(-1)(S/N=3)。结论:该法简便、快速、有效,灵敏度高,首次用于杉科植物中羟基酸的测定,取得了很好的结果。Objective：To establish an HPLC with post - column chemiluminescence method for the determination of rudimental alcohol acid in Taxodium ascendems and Taxodium distichum. Methods： The procedure was based on the chemiluminescent enhancement by alcohol acid compounds of the semicarbazide hydrochloride and KMnO4 system in a sulfuric acid medium. They could be separated on kBPCL chemiluminescence equipment and Hypersil ODS （4.6 mm × 150 mm,5 μm） column by using perchloric acid（pH =2.25） as mobile phase at a flow rate of 0. 8 mL · min^-1. Results：The calibration curves of tartaric acid, malic acid and shikimic acid was linear in the concentration ranges of 8.6 × 10^-7 -2. 6 × 10^-4 ,9.6 × 10^-8 -3 × 10^-4 and 2. 2 × 10^-7 -3.5 × 10^-3 g · mL^-1and the correlation coefficient was 0. 9991,0. 9999 and 0. 9998. The detection limit was 3. 54 × 10^ -8 ,2. 24 × 10^-9 and 2. 02 × 10^ -8 g · mL^-1（S/N = 3）. Conclusion：The method has been successfully applied to the determination of trace rudimental alcohol acid in the Taxodiaceae plant,which was proved to be accurate, high sensitivity, simple effective and feasible.

关 键 词：高效液相色谱 化学发光 杉科植物 羟基酸 

分 类 号：R917[医药卫生—药物分析学]