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目的:建立甲啶铂高效液相色谱分析方法,采用该方法测定甲啶铂原料药的纯度,并研究甲啶铂在酸碱、氧化还原环境中的稳定性。方法:采用Waters XTerra PR C18(250 mm×4.6 mm,5μm)色谱柱,以15%乙腈水溶液为流动相等度洗脱,流速1.0 m L·min-1,二极管阵列检测器(PDA)于200~400 nm内检测含量并分析纯度。在甲啶铂溶液中添加HCl、Na OH、H2O2和Na HSO3,采用高效液相色谱法测定含量,考察甲啶铂在酸碱、氧化还原环境中的稳定性。结果:此方法可以快速灵敏地测定甲啶铂含量,甲啶铂质量浓度在0.02~0.2 mg·m L-1范围内线性相关(R2>0.999 9),检测限和定量限分别为0.094 ng和0.22ng。此方法可以同时将甲啶铂与顺铂、三氯氨铂酸钾和顺式-二氯-氨、(3-甲基吡啶)合铂(Ⅱ)等杂质有效分离。纯度分析表明,试制的3批甲啶铂原料药纯度高。稳定性试验显示,碱性及氧化环境对甲啶铂具有很强的破坏作用。结论:此方法可用于甲啶铂原料药及其制备过程中的检测和监控,在甲啶铂原料药保存和制剂研究过程中应避免与碱性和氧化性物质接触。
OBJECTIVE: To establish a method for the determination of metopidium by high performance liquid chromatography (HPLC), and to determine the purity of the raw drug of metopidin. The stability of metopidium in acid-base and redox environment was also studied. METHODS: Waters XTerra PR C18 (250 mm × 4.6 mm, 5 μm) column was used to elute with a mobile phase of 15% acetonitrile at a flow rate of 1.0 mL · min-1. The PDA was operated at 200 ~ 400 nm detection of content and analysis of purity. HCl, NaOH, H2O2 and Na HSO3 were added to the solution of picoplatin, and the content of methidineplatin in acid-base and redox environment was determined by HPLC. Results: The method could rapidly and sensitively determine the content of metformin. The concentration of metopiper was linearly correlated (R2> 0.999 9) in the range of 0.02-0.2 mg · mL-1 with the limits of detection of 0.094 ng and the limits of quantitation 0.22ng. This method can effectively separate picoplatin from cisplatin, potassium cisplatin and cis-dichloro-ammonia, (3-picoline) platinum (II) and other impurities. Purity analysis showed that the trial batch of 3 copies of high purity picoplatin raw material. Stability tests showed that alkaline and oxidative environments have a strong destructive effect on the exposure to methidine. Conclusion: This method can be used for the detection and monitoring of metopidin and its preparation process. It should avoid contact with alkaline and oxidizing substances during the storage and preparation of metoplasma.