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目的探索建立改进的高效液相色谱法-梯度洗脱法检测克林霉素磷酸酯及其注射剂的有关物质。方法色谱柱为Supelco Discovery C18(4.6 mm×250 mm,5 m);流动相A为磷酸缓冲液(pH 3.9)-90%乙腈甲醇溶液(92∶8),流动相B为磷酸缓冲液(pH 3.9)-90%乙腈甲醇溶液(52∶48);柱温为40℃;检测波长为210 nm;流速为1.2 mL.min 1。结果克林霉素磷酸酯主峰与其相关物质峰分离良好,供试品中含林可霉素,克林霉素B磷酸酯,克林霉素及其他非特定杂质的量为0.006%~1.137%,0.016%~0.157%,0.005%~0.195%及0.016 3%~2.933%时,均具有良好的线性关系。林可霉素,克林霉素B磷酸酯,克林霉素以及非特定杂质(克林霉素磷酸酯)的LOD分别为0.170 5 g.mL 1,0.160 0 g.mL 1,0.146 2 g.mL 1和0.488 8 g.mL 1。林可霉素,克林霉素B磷酸酯,克林霉素各杂质的平均回收率分别104.0%(RSD=1.8%,n=9),106.8%(RSD=1.8%,n=9)和104.9%(RSD=1.8%,n=9)。结论改进方法的杂质色谱性能明显优于现行标准方法和USP个论方法,更适用于克林霉素磷酸酯及其注射剂的有关物质检测。
Objective To explore the establishment of an improved high performance liquid chromatography - gradient elution method for the determination of clindamycin phosphate and its related substances. Methods The mobile phase A was phosphate buffer (pH 3.9) -90% acetonitrile-methanol solution (92: 8) and the mobile phase B was phosphate buffer (pH 4.6) 3.9) -90% acetonitrile in methanol (52:48); the column temperature was 40 ℃; the detection wavelength was 210 nm; the flow rate was 1.2 mL.min 1. Results The main peak of clindamycin phosphate was separated from its related substances peak. The amount of clindamycin B, clindamycin B phosphate, clindamycin and other non-specific impurities was 0.006% -1.137% , 0.016% ~ 0.157%, 0.005% ~ 0.195% and 0.016 3% ~ 2.933%, respectively, all had a good linear relationship. The LOD of lincomycin, clindamycin B phosphate, clindamycin, and non-specific impurities (clindamycin phosphate) were 0.170 5 g.mL, 1, 0.1600 g.mL, 1, 0.1646 g mL 1 and 0.488 8 g.mL 1. The average recoveries of lincomycin, clindamycin B phosphate and clindamycin were 104.0% (RSD = 1.8%, n = 9), 106.8% (RSD = 1.8%, n = 9) and 104.9% (RSD = 1.8%, n = 9). Conclusion The improved impurity chromatographic performance is obviously superior to the current standard method and USP theory. It is more suitable for the detection of clindamycin phosphate and its related substances.