摘要
目的:建立测定盐酸伊立替康脂质体包封率的方法。方法:采用改进的中空纤维离心超滤法(HFCF-UF)分离脂质体和游离药物;采用高效液相色谱法测定脂质体中盐酸伊立替康的含量,色谱柱为Diamonsil C_(18),流动相为甲醇-乙腈-磷酸盐缓冲液(称取磷酸二氢钾6.8 g溶于800 mL水中,加入三乙胺10 mL,以磷酸调pH至4.0,加水定容至1 000 mL)(55∶5∶45,V/V/V),流速为1.0mL/min,检测波长为254 nm,柱温为25℃,进样量为20μL。结果:盐酸伊立替康检测质量浓度线性范围为2.55~40.8μg/mL(r=0.999 2);定量限为0.64μg/mL;中间精密度、稳定性、重复性试验的RSD均小于2%;超滤提取回收率为96.9%~100.2%(RSD=1.0%,n=9),空白加样回收率为95.5%~100.5%(RSD=1.7%,n=9)。包封率的平均值为94.85%(RSD=1.1%,n=3)。结论:该方法操作简便、准确,精密度、稳定性、重复性好,适用于盐酸伊立替康脂质体包封率的测定。
OBJECTIVE：To develop a method for determining entrapped efficiency of Irinotecan hydrochloride liposomes.METHODS：The improved hollow fiber centrifugal ultrafiltration（HFCF-UF）method was employed to separate the liposomal drug and the free drug. The content of irinotecan hydrochloride was determined by HPLC. The determination was performed on Diamonsil C（18） with mobile phase consisted of methanol-acetonitrile-phosphate buffer solution（monobasic potassium phosphate 6.8 g dissolved in 800 mL water,triethylamine 10 mL,pH adjusted to 4.0 with phosphoric acid,adding water to 1 000 mL）（55 ∶ 5 ∶ 45,V/V/V） at the flow rate of 1.0 mL/min. The detection wavelength was set at 254 nm,and column temperature was 25 ℃. The sample size was 20 μL. RESULTS：The linear range of irinotecan hydrochloride were 2.55-40.80 μg/mL（r=0.999 2）. The limit of quantitation was 0.64 μg/mL. RSDs of intermediate precision,stability and reproducibility tests were all lower than 2%. The recovery rates of ultrafiltration were 96.9%-100.2%（RSD=1.0%,n=9）, and the blank adding recovery rates ranged 95.5%-100.5%（RSD=1.7%,n=9）. The average of entrapped efficiency was 94.85%（RSD=1.1%,n=3）. CONCLUSIONS：The method is simple,accurate,precise,stable,reproducible and durable. It can be used for the determination of entrapped efficiency of Iriticonite hydrochloride liposomes.
作者
孙婷
刘彦
王晓晖
律涛
蒋晔
SUN Ting;LIU Yan;WANG Xiaohui;LYU Tao;JIANG Ye(Dept.of Clinical Pharmacology,FourthHospital of Hebei Medical University,Shijiazhuang 050011,China;School of Pharmacy,Hebei MedicalUniversity,Shijiazhuang 050017,China)
出处
《中国药房》
CAS
北大核心
2018年第16期2220-2223,共4页
China Pharmacy
基金
河北省医学科学研究重点课题(No.冀卫办科教[2017]3号-20170715)
