HPLC法测定Aβ斑块显像剂标记前体AV45的含量及有关物质
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篇名: | HPLC法测定Aβ斑块显像剂标记前体AV45的含量及有关物质 |
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摘要: | 目的:建立测定β-淀粉样蛋白(Aβ)斑块显像剂标记前体AV45的含量及有关物质的方法。方法:采用高效液相色谱法。色谱柱为Inertsil C18,流动相为50 mmol/L磷酸氢二钠溶液-乙腈(含0.01%三乙胺)(15 ∶ 85,V/V),检测波长为325 nm,流速为1.0 ml/min,柱温为30 ℃,进样量为20 μl。 结果:AV45与其反应中间体及其他杂质分离度较好;AV45及其反应中间体的检测质量浓度线性范围分别为200~1 000、20~100 μg/ml(r=0.999 2、0.999 6);AV45反应中间体的检测限、定量限分别为0.1、0.5 ng;精密度、稳定性、重复性试验的RSD<0.5%;AV45的回收率为98.93%~101.58%,RSD=0.69%(n=9)。结论:该方法简便、准确、专属性高、重复性好,适用于Aβ斑块显像剂标记前体AV45的含量及有关物质测定。 |
ABSTRACT: | OBJECTIVE: To establish a method for the content determination of AV45 (the labeled precursor of PET agent for Aβ plaques) and its related substances. METHODS: HPLC method was performed on the column of Inertsil C18 with mobile phase of 50 mmol/L Disodium hydrogen phosphate solution - acetonitrile (containing 0.01% triethylamine) (15 ∶ 85,V/V) at a flow rate of 1.0 ml/min, the detection wavelength was 325 nm, and column temperature was 30 ℃, and volume injection was 20 μl. RESULTS: The AV45 and reaction intermediate as well as individual impurity peaks were well separated; the linear range was 200-1 000 μg/ml for AV45 (r=0.999 2) and 20-100 μg/ml for intermediate (r=0.999 6); the detection limit and quantification limit of reaction intermediate AV45 were 0.1 ng and 0.5 ng, respectively; RSDs of precision, stability and reproducibility tests were lower than 0.5%; recovery of AV45 was 98.93%-101.58%(RSD=0.69%,n=9). CONCLUSIONS: The method is simple and accurate with high specificity and good reproducibility, and suitable for content determination of AV45(the labeled precursor of PET agent for Aβ plaques) and its related substances. |
期刊: | 2016年第27卷第18期 |
作者: | 毛师师,张建康,张荣军,周杏琴 |
AUTHORS: | MAO Shishi,ZHANG Jiankang,ZHANG Rongjun,ZHOU Xingqin |
关键字: | 标记前体;AV45;高效液相色谱法;含量;有关物质 |
KEYWORDS: | Labeled precursor; AV45; HPLC; Determination; Related substances |
阅读数: | 365 次 |
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