HPLC法电化学检测阿奇霉素片的有关物质

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

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。

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.