HPLC同时测定木香顺气丸中5种成分的含量  

Simultaneous Determination of Five Active Constituents in Muxiang Shunqi Pills by HPLC

作　　者：孙迪迪[1] 湛建峰 邱娟 SUN Di-di ZHAN Jian-feng QIU Juan(The Seventh People＇s Hospital of Zhengzhou, Zhengzhou 450016, China Yueyang Institute for Food and Drug Control, Yueyang 414000, China Cisen Pharmaceutical Co., Ltd, dining 272000, China)

机构地区：[1]郑州市第七人民医院,河南郑州450016 [2]岳阳市食品药品检验所,湖南岳阳414000 [3]辰欣药业股份有限公司,山东济宁272000

出　　处：《食品与药品》2017年第4期264-268,共5页Food and Drug

摘　　要：目的建立同时测定木香顺气丸中5种活性成分含量的方法。方法采用高效液相色谱法(HPLC),色谱柱为Kromasil C18柱(250 mm×4.6 mm,5μm),以乙腈为流动相A,0.2%磷酸溶液为流动相B,梯度洗脱:0~5 min,10%A;5~20 min,10%→20%A;20~40 min,20%→60%A;40~60 min,60%A;分段设定检测波长:0~20.0 min为210 nm(木香烃内酯、去氢木香内酯);20.0~30.0 min为292 nm(和厚朴酚);30.0~45.0 min为211 nm(厚朴酚);45.0~60.0 min为250 nm(甘草酸),流速1.0 m L/min,柱温30℃,进样量20μL。结果香烃内酯、去氢木香内酯、和厚朴酚、厚朴酚和甘草酸分离度良好,进样量分别在0.025~1.008,0.031~1.232,0.022~0.864,0.058~2.304,0.045~1.800μg范围内线性关系良好,r均大于0.9990,平均加样回收率为99.2%~99.7%(RSD=0.74%~1.05%)。5批样品中香烃内酯、去氢木香内酯、和厚朴酚、厚朴酚和甘草酸含量分别在6.17~6.51,2.74~2.89,13.2~13.66,2.54~2.87,4.40~4.65 mg/g。结论本方法专属性好、灵敏度高、准确度高,为木香顺气丸的质量控制提供依据。Objective To establish an HPLC method for the simultaneous determination of five active constituents in Muxiang Shunqi Pills. Methods The Kromasil C18 （250 mmx4.6 mm, 5 μm） column was used. The separation was accomplished by gradient elution, using acetonitrile （A） and 0.2 % phosphoric acid solution （B） as mobile phase： 10 % A within 0-5 min, 10 %-20 % A within 5-20 min, 20 %-60 % A within 20-40 min and 60 % A within 40- 60 rain. The detection wavelengths were set at 210 nm for costunolide and dehydrocostuslactone within 0-20.0 rain, 292 nm for honokiol within 20.0-30.0 min, 21 lnm for magnolol within 30.0-45.0 min and 250 mn for glycyrrhizic acid within 45.0-60.0 min. The flow rate was 1.0 mL/min with column temperature of 30 ℃ and injection volume of 20μL. Results The separation of Costunolide, dehydroeostuslaetone, honokiol, magnolol and glycyrrhizic acid were good. The linear ranges were 0.025-1.008 μg, 0.031-1.232 μg, 0.022-0.864 μg, 0.058-2.304 μg and 0.045-1.800 μg for costunolide, dehydrocostuslactone, honokiol, magnolol and glycyrrhizic acid, respectively, with the correlation coefficent r〉0.9990. The average recoveries varied from 99.2 % to 99.7 %, with RSD of 0.74 %-1.05 %. The contents of costunolide, dehydroeostuslactone, honokiol, magnolol and glycyrrhizic acid were 6.17-6.51 mg/g, 2.74-2.89 mg/g, 13.2-13.66 mg/g, 2.54-2.87 mg/g and 4.40-4.65 mg/g in five batches of samples, respectively. Conclusion This method has good specificity, high sensitivity and high accuracy, thus can provide scientific basis for the quality control of Muxiang Shunqi Pills.

关 键 词：木香顺气丸 HPLC 香烃内酯 去氢木香内酯 和厚朴酚 厚朴酚 甘草酸 

分 类 号：R927.2[医药卫生—药学]