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目的:建立高效液相色谱-二极管阵列检测器(HPLC-DAD)测定天然橡胶乳清中白坚木皮醇的方法。方法:鲜胶乳清用18%的乙酸凝固过滤脱胶,加0.6%滤液量的Ca(OH)_2加热煮沸脱蛋白,过滤,滤液经阴、阳离子交换树脂除去盐和类脂物,再经大孔吸附树脂吸附,60%乙醇解吸附,解吸液浓缩得结晶,溶解定容。采用Inertsil ODS-SP C_(18)色谱柱进行分离,流动相乙腈-水(10∶90),流速1.0 m L·min~(-1),柱温30℃。结果:白坚木皮醇在0.04~4.0 g·L~(-1)呈现良好的线性关系(r=0.997 9),精密度RSD 1.1%,加样回收率96.69%。结论:该方法操作简单、准确度和灵敏度高,适合于白坚木皮醇的检测和含量测定。
Objective: To establish a HPLC-DAD method for the determination of alfalfa wood in natural rubber whey. Methods: The fresh latex was degummed with 18% acetic acid coagulation and filtration. The mixture was boiled and deproteinized by adding 0.6% of the filtrate amount of Ca (OH) 2. The filtrate was filtered through a cation exchange resin to remove salts and lipids, Adsorption resin adsorption, 60% ethanol desorption, desorption solution was concentrated to crystallization, dissolved volume. The column was separated on an Inertsil ODS-SP C_ (18) column. The mobile phase was acetonitrile-water (10: 90) at a flow rate of 1.0 mL · L -1 and the column temperature was 30 ℃. Results: The linear correlation was found between 0.04 and 4.0 g · L -1 (r = 0.997 9), the RSD of precision was 1.1% and the recovery rate was 96.69%. Conclusion: The method is simple, accurate and sensitive, suitable for the determination and determination of white fir wood alcohol.