离子色谱法测定青霉胺片的含量及有关物质

目的： 建立离子色谱法测定青霉胺片的含量及有关物质。方法： 采用Dikma Spursil C₁₈（4.6 mm×250 mm，5 μm）色谱柱；流动相为5.3 g无水磷酸二氢钠和0.25 g己烷磺酸钠，加去离子水1 000 mL使溶解，用磷酸调节pH至2.85，加乙腈9 mL；流速1.0 mL·min^-1；柱后溶液为21 g·L^-1的氢氧化钠溶液；柱后流速为0.3 mL·min^-1；柱温为30℃；检测器为脉冲积分安培电化学检测器，工作电极为金电极（直径1 mm），检测电位为六电位。结果： 青霉胺质量浓度在0.049 88~0.199 5 mg·mL^-1范围内线性关系良好，回收率范围为98.4%~101.5%，含量结果为97.6%~101.5%；有关物质测定，青霉胺质量浓度在3.118~49.88μg·mL^-1范围内线性关系良好，青霉胺二硫化物质量浓度在1.616~19.39 μg·mL^-1范围内线性关系良好；青霉胺及青霉胺二硫化物检测下限均为0.02 μg，青霉胺二硫化物含量为0.4%~0.8%，最大单个杂质含量为0.9%~2.9%，其他杂质总量为2.4%~7.3%；各杂质与青霉胺峰均能完全分离。结论： 该方法准确灵敏，可用于青霉胺片的质量控制。

Objective: To establish an ion chromatography method for determination of the assay and related substances of penicillamine tablets.Methods: A Dikma Spursil C₁₈(4.6 mm×250 mm,5 μm)column was used;the mobile phase was 5.3 g of sodium dihydrogen phosphate anhydrous and 0.25 g of sodium hexane sulfonate,dissolved in 1 000 mL of deionized water,and then adjusted the pH value to 2.85 with phosphoric acid and added 9 mL of acetonitrile;the flow rate was 1.0 mL·min^-1,the post-column solution was 21 g·L^-1 sodium hydroxide solution and the flow rate was 0.3 mL·min^-1,the column temperature was 30℃;a pulsed amperometric detection was adopted,and the working electrode was gold electrode(1 mm)with a working mode of a six potential waveform.Results: Penicillamine showed good linear in the range of 0.049 88-0.199 5 mg·mL^-1,the recovery rate were 98.4%-101.5%,the assay determined were 97.6%-101.5%.Penicillamine and penicillaminedisulfide presented good linear within the range of 3.118-49.88 μg·mL^-1 and 1.616-19.39 μg·mL^-1,respectively.The detection limits of penicillamine and penicillaminedisulfide were 0.02 μg and 0.02 μg.The contents of penicillamine disulfide were 0.4%-0.8%,the contents of the largest impurities were 0.9%-2.9%,and the contents of the total impurities were 2.4%-7.3%.The related substances and penicillamine could be separated completely.Conclusion: This method is accurate and sensitive,and suitable for the quality control of penicillamine tablets.

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