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机构地区:[1]南方医科大学南方医院药学部,广州510515
出 处:《实用药物与临床》2017年第5期569-572,共4页Practical Pharmacy and Clinical Remedies
摘 要: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。Objective To develop an HPLC gradient elution method for simultaneous determination of the content of honokiol, magnolol, costnnolide and dehydrocostus lactone in Chenxiang Shuyu Pill. Methods The Phenomenex C18 ( 250 mm × 4. 6 ram,5 μm) chromatographic column 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 - 89.20μg/mL( r = 0. 999 5 ) ,5. 12 - 102.40 μg/mL( r = 0. 999 9 ), and 6. 18 - 123.60 μg/rnL( 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% ). Conduslon 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.
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