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纸质出版日期:2015
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董铁山, 王建龙, 曾日中, 等. HPLC-DAD测定天然橡胶乳清中白坚木皮醇[J]. 中国实验方剂学杂志, 2015,21(24):45-47.
DONG Tie-shan, WANG Jian-long, ZENG Ri-zhong, et al. Determination of -quebrachitol in Nature Rubber Latex Serum by HPLC-DAD[J]. Chinese journal of experimental traditional medical formulae, 2015, 21(24): 45-47.
董铁山, 王建龙, 曾日中, 等. HPLC-DAD测定天然橡胶乳清中白坚木皮醇[J]. 中国实验方剂学杂志, 2015,21(24):45-47. DOI: 10.13422/j.cnki.syfjx.2015240045.
DONG Tie-shan, WANG Jian-long, ZENG Ri-zhong, et al. Determination of -quebrachitol in Nature Rubber Latex Serum by HPLC-DAD[J]. Chinese journal of experimental traditional medical formulae, 2015, 21(24): 45-47. DOI: 10.13422/j.cnki.syfjx.2015240045.
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 C18色谱柱进行分离
流动相乙腈-水(10:90)
流速1.0 mL·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=0.9979)
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 determine L-quebrachitol in nature rubber latex serum by establishing high-performance liquid chromatography-diode array detector(HPLC-DAD). Method: Fresh latex was coagulated by 18% acetic acid and unglued by filtration. 0.6% Ca(OH)2 filtration liquid was added and heated to boiling status for removing protein
then the mixture was filtered. Salt and lipid content in the filtrate was removed by anion and cation resin exchange
and the residue achieved adsorption through macroporous adsorption resins
then desorbed by 60% ethanol
and the raw quebrachitol was obtained by Vacuum condensation crystallization. The product was dissolved in ultrapure water with metered volume. L-quebrachitol was separated by Inertsil ODS-SP C18 column with acetonitrile-water(10:90) as mobile phase at a flow rate of 1.0 mL·min-1 and column temperature of 30℃. Result: A good linear relationship was obtained in the range of 0.04-4.0 g·L-1 for L-quebrachitol
with a linear correlation coefficient(R) of 0.9979.The RSD was 1.1%
and the average recovery rate was 96.69%. Conclusion: This method is simple with high sensitivity and precision
suitable for determination of L-quebrachitol in nature rubber latex serum.
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