HPLC法同时测定没药中3个倍半萜类成分的含量

目的：建立同时测定没药中相对-1S，2S-环氧-4R-呋喃大根香叶-10（15）-烯-6-酮（化合物Ⅰ）、（1（10）E，2R，4R）-2-甲氧基-8，12-环氧大根香叶-1（10），7，11-三烯-6-酮（化合物Ⅱ）和莪术酮（化合物Ⅲ）3个倍半萜类成分含量的高效液相色谱法。方法：采用CAPCELL PAK C₁₈色谱柱（250 mm&#215;4.6 mm，5 μm），以乙腈（A）-0.1%磷酸水溶液（B）为流动相，梯度洗脱，流速1.0 mL&#183;min^-1，检测波长210 nm，柱温30℃。结果：化合物Ⅰ、Ⅱ和Ⅲ进样量分别在0.018 4~0.46 μg（r=1.000 0）、0.029~0.725 μg（r=1.000 0）和0.025 8~0.645 μg（r=1.000 0）范围内与峰面积呈现良好的线性关系，精密度（RSD<0.4%）、稳定性（rsd<0.7%）良好，平均回收率（n=6）分别为98.9%（RSD=0.48%）、98.6%（RSD=0.79%）、98.3%（RSD=0.60%）；6批样品中化合物Ⅰ、Ⅱ和Ⅲ含量范围分别为0.448~2.004、1.399~11.919和1.050~3.922 mg&#183;g^-1。结论：该方法可用于没药中化合物Ⅰ、Ⅱ和Ⅲ的含量测定。

Objective:To establish an HPLC method for the simultaneous determination of three sesquiterpenes in Commiphora myrrha,namely,rel-1S,2S-epoxy-4R-furan-ogermacr-10(15)-en-6-one(compound Ⅰ),(1(10)E,2R,4R)-2-methoxy-8,12-epoxygermacra-1(10),7,11-trien-6-one(compound Ⅱ)and curzerenone[6,7-dihydro-5β-isopropenyl-3,6β-dimethyl-6-vin-ylbenzofuran-4(5H)-one](compound Ⅲ). Methods:The CAPCELL PAK C₁₈ column(250 mm&#215;4.6 mm,5 μm)was used,the mobile phase was acetonitrile(A)-0.1% phosphate(B)with gradient elution at a flow rate of 1.0 mL&#183;min^-1. The detection wavelength was 210 nm and the column temperature was 30℃. Results:The linear ranges of compound Ⅰ,compound Ⅱ and compound Ⅲ were 0.0184-0.46 μg(r=1.000 0),0.029-0.725 μg(r=1.000 0)and 0.0258-0.645 μg(r=1.000 0),respectively. The values of precision(RSD<0.4%)and stability(RSD<0.7%)tests were good. The average recoveries(n=6)were 98.9%(RSD=0.48%),98.6%(RSD=0.79%)and 98.3%(RSD=0.60%),respectively. The contents of compound Ⅰ,compound Ⅱ and compound Ⅲ in six batches of samples were 0.448-2.004,1.399-11.919 and 1.050-3.922 mg&#183;g^-1,respectively. Conclusion:The method can be used to determine compound Ⅰ,compound Ⅱ and compound Ⅲ in Commiphora myrrha.

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