固相萃取-高效液相色谱法测定牙膏中黄芩甙

Determinztion of Baicalin in Toothpastes by Solid Phase Extraction-High Performance Liquid Chromatography

建立了固相萃取-高效液相色谱法(HPLC)检测牙膏中黄芩甙的分析方法。样品用75%乙醇超声提取20min,8 000r/min离心10min,取5mL上清液经MAX固相萃取柱处理,5%甲酸-甲醇溶液洗脱后氮吹浓缩后分析。采用ZORBAX SB C18色谱柱;流动相为乙腈-0.1%磷酸(体积比22∶78),检测波长为276nm。该方法线性范围1～100μg·mL-1,加标回收率81.3%～101.6%,检出限3.0mg·kg-1。方法准确、重现性好,干扰能力强,适用于牙膏中黄芩甙的检测。

We developed a solid phase extraction-HPLC method to determine baicalin in toothpastes. Samples were ultrasonic extracted for 20 min by 75 % alcohol and then centrifugated at 8 000 r/min for 10 min. 5 mL of supernatant wastreated by MAX solid phase extraction, eluted by 5% formic acid- methanol,and then concentrated. Finally the extracted sample was analyzed by ZORBAX SB C18 column with the mobile phase of acetonitrile：0. 1% phosphoric acid = 22：78 and detection wavelength at 276 nm. A good linear relationship was obtained from 1.00 μg-mL-1 to 100.0 μg-mL-1. The recovery of the method was in the range of 81.3%-101.6% with the limit of detection of 3.0 mg·kg 1. The established method was accurate and reproducible,and suitable for analysis of baicalin in toothpastes.