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目的:建立高效液相色谱法测定琥乙红霉素及片剂中游离红霉素,并按所建方法对全国33家企业的251批琥乙红霉素片中的游离红霉素进行测定。方法:采用SPOLAR C18(250 mm×4.6 mm,5μm)色谱柱,流动相A为磷酸二氢钾溶液(称取磷酸二氢钾3.4 g,加水适量溶解,加三乙胺2.75 m L,再以水稀释至1000 m L,用盐酸调节p H至3.0),流动相B为乙腈,线性梯度洗脱,流速为1.0 m L·min-1,柱温为30℃,检测波长为205 nm。结果:片剂辅料无干扰,线性范围为0.06~1.2 mg·m L-1,r=0.9999;检测限为0.024μg,定量限为0.12μg;平均加样回收率(n=9)为100.2%,RSD为1.3%。251批样品测定游离红霉素含量在5%以内的占65.3%;在5%~10%之间的占27.1%;大于10%的占8.0%。结论:本文建立的方法分离效果好,灵敏度高,可用于琥乙红霉素及片剂中游离红霉素的测定。有必要尽快建立HPLC方法更加准确测定琥乙红霉素及片剂中游离红霉素的含量。
OBJECTIVE: To establish a HPLC method for the determination of erythromycin ethylsuccinate and free erythromycin in tablets, and to determine the free erythromycin in 251 batches of erythromycin ethylsuccinate tablets of 33 enterprises in China according to the established method . Methods: A SPOLAR C18 (250 mm × 4.6 mm, 5 μm) column was used. The mobile phase A was potassium dihydrogen phosphate (3.4 g potassium dihydrogen phosphate, dissolved in water, 2.75 mL triethylamine, Water was diluted to 1000 mL, and pH was adjusted to 3.0 with hydrochloric acid. The mobile phase B was acetonitrile. The mobile phase B was eluted with a linear gradient at a flow rate of 1.0 mL · min-1. The column temperature was 30 ℃ and the detection wavelength was 205 nm. Results: The tablets had no interference with the linear range of 0.06-1.2 mg · m L-1, r = 0.9999. The detection limit was 0.024 μg and the limit of quantification was 0.12 μg. The average recovery was n = 9 (100.2% , RSD was 1.3%. 251 batches of samples measured free erythromycin content of less than 5% accounted for 65.3%; 5% to 10% of the 27.1%; more than 10% accounted for 8.0%. Conclusion: The method established in this paper has good separation effect and high sensitivity, which can be used to determine erythromycin ethylsuccinate and free erythromycin in tablets. It is necessary to establish an HPLC method for the more accurate determination of erythromycin ethylsuccinate and free erythromycin in the tablets as soon as possible.