基于振荡提取-C_(18)分散净化的高效液相色谱法测定蓝莓中白藜芦醇

Determination of resveratrol in blueberry by high performance liquid chromatography based on oscillating extraction-C_(18)dispersion purification

建立振荡提取-C_(18)分散净化高效液相色谱法(配二极管阵列检测器)测定蓝莓中白藜芦醇含量。试样经乙醇溶液提取和氯化钠盐析、振荡、离心。上清液经硫酸钠和C_(18)分散剂净化过微孔滤膜后待测。流动相为水和乙腈(75:25,V:V)等浓度洗脱,流速为0.7 mL/min,柱温为35℃,经色谱柱InertSustain AQ-C_(18)(4.6 mm×250 mm,5μm)分离、采用液相色谱仪配二极管阵列检测器进行全扫描检测,显示波长为306 nm,以保留时间定性,外标法定量。白藜芦醇在0.05~80.00μg/mL浓度范围内具有良好的线性关系,相关系数为0.9994,检出限为0.008 mg/kg。在0.05、1.00和2.00 mg/kg 3个添加水平下,回收率为83.6%~94.8%(n=6),相对标准偏差为1.1%~1.9%。本方法适用于蓝莓中白藜芦醇含量测定,具有简单快速、重现性好、结果准确便于推广。

To establish an analytical method for analyzing the content of resveratrol in blueberry by high performance liquid chromatography(with a diode array detector)with shock extraction and dispersion purification of C_(18)was established.The samples were extracted by ethanol solution,salted out by sodium chloride,shaken and centrifuged.The supernatant was purified by sodium sulfate and C_(18)dispersant,and collected for measurement after passing the microporous filter membrane.the mobile phase was water and acetonitrile(75:25,V:V)was used for elution at constant concentration,the flow rate was 0.7 mL/min,the column temperature was 35℃,inertSustain AQ-C_(18)(4.6 mm×250 mm,5 m)was used for separation.The full scan detection was carried out by liquid chromatography with diode array detector,the display wavelength was 306 nm,the retention time was used for the qualitative analysis,and external standard method was used for quantitative analysis.Resveratrol had a good linear relationship in the concentration range of 0.05-80.00μg/mL,correlation coefficient was 0.9994,detection limit was 0.008 mg/kg.The recoveries were 83.6%-94.8%at the supplemental levels of 0.05,1.00 and 2.00 mg/kg.Relative standard deviation was 1.1%-1.9%.Conclusion The method is suitable for the determination of resveratrol in blueberry.It has the advantages of simplicity,rapidity,good reproducibility,accurate results and easy popularization.