HPLC法电化学检测阿奇霉素片的有关物质

目的:建立以高效液相色谱法电化学检测阿奇霉素片中有关物质的方法。方法:色谱柱为Gamma ARP-1/P,流动相为0.014mol·L-1磷酸氢二钾/0.020mol·L-1氢氧化钠(用磷酸和氢氧化钠调pH至11)-乙腈(71∶29),流速为0.7mL·min-1,柱温为40℃,进样量为50μL,玻璃碳电极的检测电位为+900mV。结果:红霉素过氧化物、阿奇霉素脱氧化物、阿奇霉素杂质A和N脱甲基阿奇霉素进样量的线性范围分别为0.15~1.80(r=0.999)、0.09~1.08(r=0.999)、0.23~2.76(r=0.998)、0.30~3.60μg(r=0.998);平均回收率分别为98.9%(RSD=1.1%)、94.6%(RSD=5.4%)、103.4%(RSD=3.4%)、96.2%(RSD=4.3%),有关物质含量检测结果均<0.7%。结论:本方法重现性好、灵敏度高、结果稳定准确,可用于检测该制剂的有关物质。

Determination of the Related Substances in Azithromycin Tablet by HPLC-Electrochemical Detector

OBJECTIVE： To determine the content of the related substances in azithromycin tablet by HPLC - electro- chemical detector. METHODS： The column was Gamma ARP- 1/P. The mobile phase consisted of 0.014 mol · L^-1 dipotassium hydrogen phosphate/0.020 mol · L^-1 sodium hydroxide （pH was adjusted to 11 by phosphoric acid and sodium hydroxide） - acetonitrile （71 ： 29） at a flow rate of 0.7 mL·min^-1. The column temperature was 40℃ . The injection volume was 50μL. Glass carbon working electrode was set at ＋ 900 mV. RESULTS： The linear ranges of erythromycin peroxide, deoxyazithromycin, azithromycin impurity A, and N - demethlation azithromycin were 0.15- 1.80μg （ r = 0. 999）, 0.09- 1.08 μg （r=0.999）, 0.23-2.76μg （r=0.998） and 0.30-3.60μg （r=0.998）, respectively. The average recoveries were 98.9% （RSD=1.1%）, 94.6% （RSD=5.4%）, 103.4% （RSD=3.4%） and 96.2% （RSD= 4.3% ）, respectively. The contents of the related substances were all below 0.7% . CONCLUSION： The established method is reproducible, sensitive and reliable, and applicable for the detection of the related substances in azithromycin tablets.