医学论文范文:RPHPLC法测定温肾苏拉甫片中吗啡的含量
【摘要】 目的:以温肾苏拉甫片为研究对象,建立对罂粟壳中所含吗啡的含量测定方法。方法: 采用RPHPLC法:SHIMADZUPack VPODS 色谱柱(4.6×150 mm,5 μm),流动相为甲醇-乙腈-0.5%醋酸铵溶液-三乙胺(12.5∶12.5∶75∶0.06),流速1.0 ml/min,检测波长为287 nm,柱温:35℃,进样量:10 μl。结果:吗啡在21.8~436.0 μg/ml浓度范围内呈良好的线性关系(r=0.999 7,n=5);平均回收率低、中、高浓度分别为:96.99%、97.55%、100.17%,相应的RSD值分别为:0.52%、0.37%、0.33%(n=9)。供试液稳定性日内和日间RSD分别为:0.80%、0.89%。最小检测限为0.72 μg/ml。结论:本方法专属性强、操作简单、灵敏度高、结果准确、重现性好,可用于制剂的质量控制,同时完善并提高了原有的药品质量标准。
【关键词】 RP HPLC 温肾苏拉甫片 吗啡
Determination of morphine content in compound tablets by RPHPLC
YAN Huan, ZHONG Jie, YAN Ming, et al
(Xinjiang Institute of Materia Medica, Urumqi 830004, China)
Abstract: Objective: To develop an RPHPLC method for determination morphine content in compound tablets. Methods: By RPHPLC. The liquid chromatography was carried out using a SHIMADZUPack VPODS column (4.6×150 mm, 5 μm). The flow rate of the mobile phase: methanolacetonitrile 0.5% ammonium acetatetriethylamine (12.5∶12.5∶75∶0.06) was 1.0 ml/min. Detection wavelength was at 287 nm, column temperature was at 35℃, the injection volume was 10 μl. Results: The linear response range of morphine was 21.8~436.0 μg/ml (r=0.999 7, n=5). The average recovery was not less then 96.99%, RSD was less then 0.33% (n=9). The RSD for interday and intraday were all less then 0.80% (n=6). Detectable concentration limited was 0.72 μg/ml. Conclusion: The method is simple, sensitive, accurate and reproducible. It can be used in quality control of Wenshensulafu compound tablets.
Key words: RPHPLC; compound tablets; morphine
温肾苏拉甫片为新疆地方标准维药,其主要成分有中亚白及、肉豆蔻、高良姜、附子、肉豆蔻衣、肉桂、罂粟壳、西红花等[1-2]。该方的原质量标准方法简单,又因罂粟壳所含的主要生物活性成分为吗啡类生物碱,归属于麻醉药品,连续使用易产生身体依赖性,能成瘾癖,吗啡是罂粟壳中含量最大的毒性成份,致死量为100 mg,极量为30 mg。可待因是罂粟壳中另一毒性成分,仅为吗啡毒性的1/8。罂粟碱对人的致死量为100~500 mg,由此可见控制罂粟壳的毒性主要是控制吗啡的含量,这是建立吗啡的含量测定方法和规定毒限的依据。本文主要以HPLC法对吗啡及罂粟碱进行含量测定,方法简便、重现性好,结果准确可靠,与其它分析方法比照,结果甚为满意医.学.全.在.线www.lindalemus.com。
1仪器与试剂
仪器:LC2010C日本岛津(SHIMADZU)高效液相色谱仪(ODS柱:150 mm×4.6 mm);CLASSVP色谱工作站。温肾苏拉甫片(新疆华康药业有限责任公司提供);硫酸吗啡标准品(批号:12380103),由中国药品生物制品检定所提供。试剂均系分析纯(西安化学试剂厂提供)。实验药材均由自治区维吾尔医医院提供。