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目的:建立同时测定板蓝根药材中水杨酸、丁香酸、苯甲酸和邻氨基苯甲酸含量的高效毛细管电泳方法。方法:采用重力进样,进样高度10 cm,进样时间30 s,正极进样,负极柱上220 nm检测。操作电压11.5 kV,运行缓冲溶液为乙腈-硼砂(15%乙腈,25 mmol·L~(-1)硼砂,15 mmol·L~(-1)β-CD),pH 9.10。对电压、缓冲液pH、缓冲液浓度、乙腈、β-CD浓度等因素对分离的影响做了系统的研究。水杨酸、丁香酸、苯甲酸和邻氨基苯甲酸分别在3.0~90,4.0-120,2.0~60,5.0~100 mg·L~(-1)线性关系良好(r=0.999 4,0.999 5,0.999 8,0.999 2);回收率分别为95.9%~102.6%,98.6%~103.4%,98.7%~104.1%,96.1%~104.3%,基于3倍信噪比(S/N=3),4种有机酸的检出限分别为0.7,1.1,1.2,1.5mg·L~(-1)。
Objective: To establish a high performance capillary electrophoresis method for the simultaneous determination of salicylic acid, syringic acid, benzoic acid and anthranilic acid in Radix Isatidis. Methods: Using gravity injection, the injection height was 10 cm, the injection time was 30 s, the positive sample was taken and the negative sample was detected at 220 nm. The operating voltage was 11.5 kV. The running buffer solution was acetonitrile-borax (15% acetonitrile, 25 mmol·L -1 borax, 15 mmol·L -1 β-CD) at pH 9.10. The effects of voltage, buffer pH, buffer concentration, acetonitrile, β-CD concentration on the separation were studied systematically. Salicylic acid, syringic acid, benzoic acid and anthranilic acid showed good linearity (r = 0.999 4,0.999 5) at 3.0 ~ 90,4.0-120,2.0 ~ 60,5.0 ~ 100 mg · L -1 , 0.999 8,0.999 2). The recoveries were 95.9% -102.6%, 98.6% -103.4%, 98.7% -104.1% and 96.1% -104.3% respectively. Based on the 3 times S / N ratio The detection limits of four organic acids were 0.7, 1.1, 1.2 and 1.5 mg · L -1, respectively.