反相高效液相色谱法测定乌腺金丝桃中伪金丝桃素的含量  

RP-HPLC Determination of Pseudohypericin in Hypericum Attenuatum Choisy

作　　者：宋海燕[1,2] 梁丽青 程振玉[4] 张克勤[1,2] 

机构地区：[1]吉林农业科技学院实验管理中心,吉林132101 [2]长白山动植物资源利用与保护吉林省高校重点实验室,吉林132101 [3]吉林农业科技学院水利与土木工程学院,吉林132101 [4]吉林化工学院化学与制药工程学院,吉林132022

出　　处：《理化检验（化学分册）》2017年第10期1161-1166,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：吉林农业科技学院科学技术项目(119012015008)

摘　　要：样品(10.000 0 g)经80%(体积分数)乙醇溶液300 mL于70℃下超声提取35 min(超声功率225 W)。分取浓缩后的提取液总质量的10%,用80%乙醇溶解并定容至100 mL,经0.45μm PTEF微孔滤膜过滤后,进行反相高效液相色谱分离。以VP-ODS C18色谱柱为固定相,以不同体积比的0.006 mol·L-1的磷酸氢二钠-磷酸溶液(p H 6.5)和甲醇的混合液为流动相进行梯度洗脱。伪金丝桃素的质量浓度在0.21~200.0 mg·L-1的范围内与其峰面积呈线性关系,检出限为(3S/N)为0.040 mg·L-1。按标准加入法进行回收试验,回收率为95.3%~101%,测定值的相对标准偏差(n=6)均小于3.5%。The sample （10. 000 0 g） was extracted ultrasonically for 35 rain with 300 mL of 80% （φ） ethanol solution at 70 ℃ （Ultrasonic power 225 W）. An aliquot of 10% of total mass of the concentrated extract was dissolved and made its volume up to 100 mL with 80% ethanol, and filtered through 0. 45 μm PTEF microporous filter membrane. The diluted solution was separated by RP-HPLC using VP-ODS C18 chromatographic column as the stationary phase and a mixture of 0. 006 mol ·L^-1 disodium hydrogen phosphate-phosphoric acid solution （pH 6. 5） and methanol in various ratios as mobile phase in gradient elution. Linear relationship between values of peak area and mass concentration of pseudohypericin was found in the range of 0. 21- 200. 0 mg·L^-1 , with detection limit （3S/N） of 0. 040 mg ·L^-1. Test for recovery was made by standard addition method, .giving results in the range of 95.3%-101%, with RSDs （n=6） all less than 3. 5%.

关 键 词：反相高效液相色谱法 超声提取 乌腺金丝桃 伪金丝桃素 

分 类 号：O652.63[理学—分析化学]