HPLC法同时测定沉香舒郁丸中四种成分的含量

目的建立波长切换联合梯度洗脱HPLC法同时测定沉香舒郁丸中和厚朴酚、厚朴酚、木香烃内酯和去氢木香内酯4个成分的含量。方法采用Phenomenex C_(18)(250 mm×4.6 mm,5μm),以甲醇(A)-0.5%磷酸溶液(B)为流动相,进行梯度洗脱,流速0.9 mL/min,检测波长:294 nm(和厚朴酚、厚朴酚),225 nm(木香烃内酯、去氢木香内酯),柱温30℃,进样量10μL。结果和厚朴酚、厚朴酚、木香烃内酯和去氢木香内酯4个成分的质量浓度分别在4.30~86.00μg/mL(r=0.999 8)、4.46~89.20μg/mL(r=0.999 5)、5.12~102.40μg/mL(r=0.999 9)、6.18~123.60μg/mL(r=0.999 2)范围内与峰面积呈良好的线性关系;平均加样回收率及相应的RSD分别为98.57%(1.08%)、99.93%(0.73%)、97.26%(1.24%)、97.65%(0.99%);重复性良好,RSD≤1.75%;精密度良好,RSD≤1.06%。供试品溶液在室温条件下24 h内稳定,RSD≤1.11%。平均加样回收率在97.26%~99.93%,RSD≤1.24%。结论所建立的方法专属性好,准确度高,灵敏度高,快速,为沉香舒郁丸的质量控制提供依据。

Simultaneous determination of the content of four constituents in Chenxiang Shuyu Pill by HPLC

Objective To develop an HPLC gradient elution method for simultaneous determination of the content of honokiol,magnolol,costunolide and dehydrocostus lactone in Chenxiang Shuyu Pill.Methods The Phenomenex C18 (250 m ×4.6 mm,5μm) chromatographic colum was adopted;the mobile phase was methanol(A)0.5％ phosphoric acid solution (B) with gradient elution,at a flow rate of 0.9 mL/min;honokiol and magnolol were detected at 294 nm,and costunolide and dehydrocostus lactone were detected at 225 nm;the column temperature was set at 30 ℃,and sample quantity was 10 μL.Results Honokiol,magnolol,costunolide and dehydrocostus lactone has a good linear relationship with peak area within the scope of concentration of 4.30 ～ 86.00 μg/mL (r =0.999 8),4.46 ～ 89.20 μg/mL(r =0.999 5),5.12 ～ 102.40 μg/mL(r =0.999 9),and 6.18 ～ 123.60 μg/mL (r =0.999 2).The average recoveries and the corresponding RSD were 98.57％ (1.08％),99.93％ (0.73％),97.26％ (1.24％)and 97.65％ (0.99％),respectively;the repeatability was good,RSD≤1.75％;the precision was good,RSD≤1.06％.Test solution was stable at room temperature within 24 h,RSD≤1.11％.The recovery rate was 97.26％ ～99.93％ (RSD≤ 1.24％).Conclusion The established method is of good specificity,high accuracy,high sensitivity and rapidity,which can be applied to the quality control of Chenxiang Shuyu Pill.