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

作　　者：陈馥[1] 周颖仪[1] 李华[1] 聂黎行[2] 戴忠[2] 马双成[2] CHEN Fu;ZHOU Ying-yi;LI Hua;NIE Li-xing;DAI Zhong;MA Shuang-cheng(Guangdong Institute for Drug Control,Guangzhou 510700,China;National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]广东省药品检验所,广州510700 [2]中国食品药品检定研究院,北京100050

出　　处：《药物分析杂志》2019年第10期1771-1780,共10页Chinese Journal of Pharmaceutical Analysis

基　　金：广东省省级科技计划项目（2018B020207008）;广东省科技厅粤港合作项目（2017A050506034）;中国食品药品检定研究院学科带头人培养基金资助项目(2017X1)

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0.25μm),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,5μm),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20μL;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,2.7μm),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2μL。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。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 determinationof 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 m L·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 m L·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,pogos

关 键 词：沉香化气丸 对照制剂 多组分含量测定 乙酸龙脑酯 百秋李醇 吉马酮 去氢木香内酯 沉香四醇 甘草苷 芸香柚皮苷 橙皮苷 甘草酸 木香烃内酯 广藿香酮 气相色谱法 高效液相色谱法 超高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]