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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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基于对照制剂的沉香化气丸多组分含量测定研究

Study on multi-component determination of Chenxiang Huaqi pills based on reference drug

分类号:R917
出版年·卷·期(页码):2019,39 (10):1771-1780
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:建立沉香化气丸的多组分含量测定方法;研制沉香化气丸对照制剂,随行测定,并将其用于质量评价。方法:采用GC法测定乙酸龙脑酯、百秋李醇、吉马酮、去氢木香内酯4个成分的含量,使用DB-17毛细管柱(30 m×0.25 mm,膜厚度为0.25 μm),程序升温,进样口温度为200℃,检测器(FID)温度为250℃,分流比为5∶1;采用HPLC法测定沉香四醇的含量,使用Phenomenex Luna C18色谱柱(4.6 mm×250 mm,5 μm),以乙腈(A)-0.1%甲酸溶液(B)为流动相,梯度洗脱,检测波长252 nm,流速1 mL·min-1,柱温40℃,进样量20 μL;采用UPLC波长切换法同时测定甘草苷、芸香柚皮苷、橙皮苷、甘草酸、木香烃内酯和广藿香酮6个成分的含量,使用Phenomenex Kinetex C18色谱柱(4.6 mm×100 mm,2.7 μm),以乙腈(A)-0.1%磷酸水溶液(B)为流动相,梯度洗脱,分段变波长测定,流速0.8 mL·min-1,柱温35℃,进样量2 μL。研制沉香化气丸对照制剂,随行测定,并将其用于质量评价。结果:对照制剂中的沉香四醇、百秋李醇、甘草苷、芸香柚皮苷、橙皮苷、甘草酸、去氢木香内酯和木香烃内酯的总量、广藿香酮含量分别为0.150、0.39、0.33、0.82、5.53、0.88、1.17、0.20 mg·g-1;37批样品中百秋李醇、甘草苷、芸香柚皮苷、橙皮苷、甘草酸、去氢木香内酯和木香烃内酯的总量、广藿香酮的含量测定结果分别为0.02~0.20、0.18~0.75、0.49~3.03、4.13~12.26、0.38~0.86、0.28~2.75、0.13~0.33 mg·g-1,4家生产企业的37批样品均有组分未能达到拟定的含量限度(百秋李醇、沉香四醇、甘草苷、橙皮苷、甘草酸、去氢木香内酯和木香烃内酯的总量、广藿香酮、芸香柚皮苷的含量限度分别为0.11、0.030、0.21、1.67、0.67、0.53、0.10、0.41 mg·g-1),22批样品未检出沉香四醇。结论:所建方法准确、简便、客观,可更加全面地控制沉香化气丸的质量。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To establish a multi-component determination method for Chenxiang Huaqi pills.Chenxiang Huaqi pills reference drug was developed and used for quality evaluation.Methods: GC method for the determination of bonyl acetate,patchouli alcohol,germacrone and dehydrocostus lactone in Chenxiang Huaqi pills was performed on a DB-17 capillary column (30 m×0.25 mm,0.25 μm)with temperature programming.Temperature of the inlet and the detector were 200℃ and 250℃,respectively.The split ratio was 5:1.HPLC method for the determination of agarotetrol was performed on a Phenomenez Luna C18 column (4.6 mm×250 mm,5 μm),with gradient elution of acetonitrile (A)-0.1% formic acid.The detection wavelength was 252 nm,the flow rate was 1 mL·min-1,the column temperature was 40℃,and the injection volume was 20 μL.UPLC with wavelength switching method for the determination of liquiritin,narirutin,hesperidin,glycyrrhizicacid,costunolide and pogostone in Chenxiang Huaqi pills was performed on a Phenomenex Kinetex C18 column (4.6 mm×250 mm, 5 μm)with gradient elution of acetonitrile and 0.1% phosphoric acid at a flow rate of 0.8 mL·min-1.The column temperature was 40℃ and the injection volume was 20 μL.Results: Contents of agarotetrol,patchouli alcohol,liquiritin,narirutin,hesperidin,glycyrrhizic acid,total content of dehydrocostus lactone and costunolide,and pogostone in reference drug were 0.150,0.39,0.33,0.82,5.53,0.88,1.17 and 0.20 mg·g-1,respectively.The contents in 37 samples were in the ranges of 0.02-0.20 mg·g-1 for patchouli alcohol,0.18-0.75 mg·g-1 for liquiritin,0.49-3.03 mg·g-1 for narirutin,4.13-12.26 mg·g-1 for hesperidin,0.38-0.86 mg·g-1 for glycyrrhizic acid,0.28-2.75 mg·g-1 for dehydrocostus lactone and costunolide and 0.13-0.33 mg·g-1 for pogostone,respectively.37 samples from four manufacturers failed to reach the proposed limits (the proposed limits for patchoulialcohol,agarotetrol,liquiritin,hesperidin,glycyrrhizic acid,total content of dehydrocostus lactone and costunolide,pogostone and narirutin were 0.11,0.030,0.21,1.67,0.67,0.53,0.10 and 0.41 mg·g-1,respectively),and agarotetrol was not detected in 22 samples.Conclusion: The proposed methods are accurate,simple and objective,which offer a more comprehensive approach for quality control of Chenxiang Huaqi pills.

-----参考文献:---------------------------------------------------------------------------------------

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