摘要
目的完善降脂舒心合剂的质量控制标准。方法以Waters XB C18(4.6 mm×250 mm,5μm)为色谱柱,以甲醇为流动相A,以混合水溶液(含磷酸为0.6%和四氢呋喃0.2%)为流动相B。梯度洗脱:0~15 min,2%A;15~55 min,2%~25%A;55~90 min,25%~40%A;90~110 min,40%~50%A。检测波长为280 nm,柱温30℃,流速为1.0 mL/mim,分析时间为120 min,进样量为10μL。采用上述方法建立降脂舒心合剂的指纹图谱。采用高效液相色谱法对该制剂中防腐剂的含量进行测定。采用电感耦合等离子质谱法对其可能含有的重金属及有害元素进行检测。结果 10批样品相似度均符合要求;苯甲酸含量均<0.3%。样品铅、镉、铬、砷、镍、铜、汞含量均符合《美国药典》新通则<232>的规定。结论本研究建立的指纹图谱简便、重复性好,为降脂舒心合剂的综合质量评价提供了科学依据;建议增加影响制剂安全性的项目,以便严格控制制剂质量。
Objective To improve the quality control standard of Jiangzhi Shuxin Mixture.Methods Waters XB C18(4.6 mm×250 mm,5μm)was used as the mobile phase,and methanol was used as mobile phase A.The mixed aqueous solution(containing 0.6%phosphoric acid and 0.2%tetrahydrofuran)was used as mobile phase B.Gradient elution:0-15 min,2%A;15-55 min,2%-25%A;55-90 min,25%-40%A;90-110 min,40%-50%A.The detection wavelength was 280 nm,the column temperature was 30℃,the flow rate was 1.0 mL/mim,the analysis time was 120 min,and the injection volume was 10μL.The above method was used to establish a fingerprint for Jiangzhi Shuxin Mixture.The content of the preservative in the preparation was determined by high performance liquid chromatography.Inductively coupled plasma mass spectrometry is used to detect heavy metals and harmful elements that may be contained.Results The similarity of 10 batches of samples met the requirements.The contents of benzoic acid were less than 0.3%.The contents of lead,cadmium,chromium,arsenic,nickel,copper and mercury in the samples all conform to the new general rule<232>of the American Pharmacopoeia.Conclusion The fingerprint established in this study is simple,reproducible and provides a scientific basis for the comprehensive quality evaluation of Jiangzhi Shuxin Mixture.It is suggested that more items affecting the safety of the preparation should be added in order to strictly control the quality of the preparation.
作者
刘敏
范蕾
陈桂云
余乐
冯美玲
LIU Min;FAN Lei;CHEN Guiyun;YU Le;FENG Meiling(Lishui Institute of Food and Drug & Quality and Technical Inspection,Zhejiang Province,Lishui 323000,China)
出处
《中国医药导报》
CAS
2019年第9期117-122,共6页
China Medical Herald
基金
浙江省食品药品监督管理与产业发展研究会课题(ZYH2016010)
关键词
降脂舒心合剂
指纹图谱
防腐剂
重金属及有害元素
Jiangzhi Shuxin Mixture
Fingerprint
Antiseptic
Heavy metals and harmful elements
作者简介
刘敏(1983-),女,硕士,副主任中药师;研究方向:中药质量控制及分析方法。
