摘要
目的:建立人体血浆中阿奇霉素 HPLC 测定法。方法:血样采用固相萃取方法,即2.0 mL 血浆过柱抽干后,用1.0 mL双蒸水连续淋洗2次,淋洗液弃去,再用1.0 mL 甲醇洗脱回收,回收液于60℃水浴挥干,最后用100 μL流动相溶解残渣,取30 μL进样。流动相为0.03 mol·L^(-1)磷酸二氢钾缓冲液(pH=4.5)-甲醇-乙腈(72:18:10);流速为1.0 mL·min^(-1);色谱柱为 C_(18)柱(4.6 mm×250 mm,5μm);柱温为室温;检测波长为210 nm。结果:阿奇霉素在0.01~1.44 mg·L^(-1)范围内线性关系良好(r=0.9994),最低检测浓度为0.008 mg·L^(-1),方法回收率在98.6%~104.4%,日内、日间 RSD 均小于5.6%。结论:该方法快速、灵敏、准确,可用于人体血浆中阿奇霉素浓度的测定。
Objective: To develop an HPLC assay for the determination of azithromycin in human plasma. Method: 2. 0 mL plasma sample was applied to C18 cartridges. After washing with 2. 0 mL water,the cartridge was eluted with 1.0 mL methanol. The eluate was evaporated to dryness at 60 ℃. The residue was dissolved in mobile phase and injected onto a Diamonsil ODS column (4. 6 mm × 150 mm,5 μm). The mobile phase was 0. 03 mol · L^-1 KH2PO4 (pH =4. 5 ) - methanol - acetonitrile (72: 18: 10). The flow rate was 1.0 mL · min^-1. An ultraviolet detector was set at 210 nm wavelength to monitor eluted components. Result:The linear range of azithromycin was 0. 01 - 1.44 mg · L^-1, r = 0. 9994. The low limit of detection was 0. 008 mg · L^-1. The method recovery was 98.6% - 104. 4%. Within- day precision (RSD) and between- day precision (RSD) were less than 5.6%. Conclusion: The assay is rapid, sensitive and accurate for the determination of azithromycin in human plasma.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2007年第2期174-176,共3页
Chinese Journal of Pharmaceutical Analysis