反相高效液相色谱法测定甲泼尼龙琥珀酸钠注射液含量和有关物质

目的: 建立甲泼尼龙琥珀酸钠注射液含量以及有关物质的反相高效液相色谱检测方法。 方法: 采用Zorbax-XDB-C₁₈柱(100 mm×46.mm,5 μm),流动相为0.66%四丁基氢氧化铵溶液(磷酸调pH至6.5)-乙腈(3∶2),流速1.0 mL·min^-1,检测波长为254 nm。 结果: 甲泼尼龙琥珀酸在100~900 μg·mL^-1浓度范围内线性关系良好(r=1.0000),高、中、低3种不同浓度的回收率分别为100.7%,100.5%,100.7%,定量限0.5 μg·mL^-1,游离甲泼尼龙在10-50 μg·mL^-1浓度范围内线性关系良好(r=1.0000),高、中、低3种不同浓度回收率分别为100.5%,100.6%,100.3%,检测限0.05 μg·mL^-1。 结论: 本方法将现有的正相色谱法改进为反相色谱法。操作简便,精密度好,结果准确可靠,可用于该制剂的质量控制。

Objective: To establish an RP-HPLC method for determination of methylpredisolone succinate injection and its related substunces. Method: Zorbax-XDB-C₁₈ column(100 mm×4.6 mm,5 μm) was used.Mobile phase was 0.66% tetrabutylammonium hydroxide solution(pH was adjusted to 6.5 by phosphoric acid)-acetonitrile(3∶2),the flow rate was 1.0 mL·min^-1and the detection wavelength was 254 nm. Results: Calibration curve of methylpredisolone succinate was linear range of 100-900 μg·mL^-1(r=1.00000),and the average recoveries of its high,middle and low concentrations were 100.7%,100.5% and 100.7%,respectively.Calibration curve of methylpredisolone was linear range of 10-50 μg·mL^-1(r=0.99995),and the average recoveries of its high,middle and low concentrations were 100.5%,100.6% and 100.3%,respectively. Conclusions: The RP-HPLC method is employed instead of the former NP-HPLC.This method is accurate and reliable,so it can be used for quality control of methylpredisolone sodium succinate injection.

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