UV法或HPLC法结合金属离子沉淀法测定米索硝唑pH敏感脂质体中主成分含量的比较
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篇名: UV法或HPLC法结合金属离子沉淀法测定米索硝唑pH敏感脂质体中主成分含量的比较
TITLE:
摘要: 目的:建立测定米索硝唑pH敏感脂质体中主成分含量的方法。方法:采用金属离子沉淀法(以ZnCl2为金属离子沉淀剂)预处理除去米索硝唑pH敏感脂质体中的辅料磷脂酰乙醇胺;采用紫外分光光度法(UV)测定其中主成分的含量(检测波长为322 nm),并将测定结果与高效液相色谱法(HPLC)进行比较[色谱柱为Hypersil C18,流动相为甲醇-水(20 ∶ 80,V/V),流速为1.0 mL/min,检测波长为322 nm,柱温为30 ℃,进样量为20 μL]。结果:两种方法检测米索硝唑的质量浓度线性范围分别为0.96~30.72 μg/mL(r=0.999 6)、0.48~4.80 μg/mL(r=0.999 5);精密度、稳定性、重复性试验的RSD均小于2%;回收率分别为97.23%~102.33%(RSD=1.05%,n=9)、97.35%~99.75%(RSD=1.15%,n=9);含量测定结果分别为99.86%、100.16%、100.32%和99.95%、99.98%、100.05%。结论:UV法结合金属离子沉淀法操作简便、准确,精密度、稳定性、重复性好,可用于米索硝唑pH敏感脂质体中主成分的含量测定,其结果与HPLC法含量测定结果一致。
ABSTRACT: OBJECTIVE: To establish the method for the determination of main components in Misonidazole pH-sensitive liposome. METHODS: The phosphatidylethanolamine in Misonidazole pH-sensitive liposomes was removed by metal ion precipitation method (using ZnCl2 as the metal ion precipitating agent). The content of main components was determined by UV spectrometry (at the wavelength of 322 nm), and then compared with the results of HPLC method [Hypersil C18, mobile phase consisted of methanol-water (20 ∶ 80, V/V), flow rate of 1.0 mL/min, detection wavelength of 322 nm, column temperature of 30 ℃, sample size of 20 μL]. RESULTS: The linear range of misonidazole were 0.96-30.72 μg/mL (r=0.999 6) and 0.48-4.80 μg/mL (r=0.999 5) by two methods. RSDs of precision, stability and reproducibility tests were all lower than 2%. The recovery rates were 97.23%-102.33% (RSD=1.05%,n=9) and 97.35%-99.75% (RSD=1.15%,n=9). The contents were 99.86%, 100.16%, 100.32% and 99.95%, 99.98%, 100.05%. CONCLUSIONS: UV method combined with metal ion precipitation method is simple, accurate, species, stable, and reproducible. It can be used for the determination of misonidazole content in misonidazole pH-sensitive liposome. The result is in agreement with those determined by HPLC.
期刊: 2018年第29卷第24期
作者: 魏巍,何美,王琛,李睿,李必波,罗治彬
AUTHORS: WEI Wei,HE Mei,WANG Chen,LI Rui,LI Bibo,LUO Zhibin
关键字: 米索硝唑;pH敏感脂质体;紫外分光光度法;高效液相色谱法;金属离子沉淀法;含量测定
KEYWORDS: Misonidazole; pH-sensitive liposome; UV spectrometry; HPLC; Metal ion precipitation method; Content determination
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