乳腺炎冲剂质量标准研究  

Study on quality standard of Mastitis Granules

作　　者：段松冷[1] 刘敏 刘礼斌 刘俊丽 田佳懿 曾蔚欣[1] DUAN Songleng;LIU Min;LIU Libin;LIU Junli;Tian Jiayi;ZENG Weixin(Department of Pharmacy,Beijing Shijitan Hospital,Capital Medical University,Beijing 100038,China;Beijing Key Laboratory of Bio-characteristic Profiling for Evaluation of Clinical Rational Drug Use,Beijing 100038,China;International Cooperation&Joint Laboratory of Bio-characteristic Profiling for Evaluation of Rational Drug Use,Bei-jing 100038,China;不详)

机构地区：[1]首都医科大学附属北京世纪坛医院药剂科,北京100038 [2]临床合理用药生物特征谱学评价北京市重点实验室,北京100038 [3]临床合理用药生物特征谱学评价国际合作联合实验室,北京100038 [4]不详

出　　处：《中国医药导报》2019年第36期111-114,共4页China Medical Herald

基　　金：国家“重大新药创制”科技重大专项（2017ZX09301040）

摘　　要：目的建立乳腺炎冲剂质量标准。方法高效液相色谱(HPLC)法测定乳腺炎冲剂中芍药苷含量。采用Agi-lent EClipse SB-C 18色谱柱(4.6 mm×250 mm,5μm),甲醇-0.05 mol/L磷酸二氢钾溶液(40∶60)为流动相,流速为1.0 mL/min,检测波长230 nm,柱温30℃,进样量10μL;薄层色谱鉴别乳腺炎冲剂中香附、当归和赤芍;重金属检查法和砷盐检查法测定乳腺炎冲剂中重金属和砷盐限度。结果HPLC法测定芍药苷含量:芍药苷质量浓度在5.01~501μg/mL(r=0.9996)范围内与峰面积呈良好的线性关系,平均回收率为99.92%,RSD=1.26%(n=6);薄层色谱法:样品斑点清晰,无阴性干扰;乳腺炎冲剂重金属和砷盐限度检查,结果符合规定。结论HPLC法测定结果准确、灵敏度高、重复性好;薄层色谱法操作简便,试验周期短,结果清晰可靠;现行药典中重金属和砷盐检查法可以用于乳腺炎冲剂重金属和砷盐的的限度检查,以上方法为建立乳腺炎冲剂治疗标准提供了依据。Objective To establish the quality standard of Mastitis Granules.Methods Paeoniflorin content in Mastitis Granules was determined by high performance liquid chromatography(HPLC).Agilent EClipse SB-C18 column(4.6 mm×250 mm,5μm)was used as the column,methanol-0.05 mol/L potassium dihydrogen phosphate solution(40∶60)was used as the mobile phase,the volume flow rate of 1.0 mL/min,with the detection wavelength of 230 nm.The colomn temperature maintained at 30℃.The injection volume was 10μL.The identification of Cyperus rotundus L.,Angelica sinensis and Paeoniae Radix Rubra in Mastitis Granules were determined by thin-layer chromatography(TLC).The limits of heavy metals and arsenic salts in Mastitis Granules were determined by heavy metal test method and arsenate test separately.Results The content of paeoniflorin was determined by HPLC.The paeoniflorin in the range of 5.01-501μg/mL(r=0.9996)showed a good linear relationship with the peak area.The average recovery rate was 99.92%,RSD=1.26%(n=6).The spots of TLC samples were clear and there was no negative interference,the limit tests of heavy metals and arsenic salts in Mastitis Granules were in accordance with the regulations.Conclusion The results of determination by HPLC are accurate,sensitive and reproducible.TLC method is simple and easy to op-erate,with short test period and clear and reliable results.The current pharmacopoeia method for heavy metals and ar-senic salts can be used for the limit examination of heavy metals and arsenic salts in Mastitis Granules.The above methods provide a basis for establishing the treatment standard of Mastitis Granules.

关 键 词：乳腺炎冲剂 质量标准 高效液相色谱法 薄层色谱 重金属砷盐限度检查 

分 类 号：R282[医药卫生—中药学]