氟腺嘌呤溶液剂的制备及其浓度测定  

Preparation and determination of arprinocid solution

作　　者：严明[1] 张丽芳[2] 薛飞群[2] 王霄旸[2] 吴昊[1] 张崇[1,2] 江善祥[1] 

机构地区：[1]南京农业大学动物医学院,江苏南京210095 [2]中国农业科学院上海兽医研究所,上海201100

出　　处：《南京农业大学学报》2014年第3期107-111,共5页Journal of Nanjing Agricultural University

基　　金：国家863计划项目(2011AA10A214)

摘　　要：为开发氟腺嘌呤新制剂并建立其浓度测定的方法,采用单因素正交设计试验法筛选出氟腺嘌呤溶液剂最优配方,采用高效液相色谱法（HPLC）测定溶液剂浓度。筛选出氟腺嘌呤溶液剂各因素最佳组合为溶媒用量为40%、助溶剂用量为50%、抗氧剂用量为0.2%、pH值约为3.0。建立的HPLC色谱条件为色谱柱Diamonsil C18（4.6 mm×250 mm,5.0μm）,流动相乙腈-水（0.1%磷酸＋0.1%三乙胺）的体积比为18∶82,流速1.0 mL·min-1,柱温30℃,紫外检测波长261 nm,进样体积10μL。辅料干扰试验显示氟腺嘌呤在出峰位置不受辅料干扰,专属破坏试验表明与降解产物均能分开。在50～100μg·mL-1的浓度范围内,峰面积（y）与药物质量浓度（x）呈良好线性关系（R2=0.999 3,n=5）,回归方程为y=34 772x＋14 371,精密度试验相对标准偏差（RSD）为0.4%（n=6）,在80、100和120μg·mL-13个添加水平时,平均回收率为98.56%（RSD=0.53%）,定量限和检测限分别为64和24 ng·mL-1,溶液剂平均浓度为40.08 mg·mL-1,平均标示含量为100.19%。该处方合理、制备工艺可靠,所建立的高效液相色谱法可用于氟腺嘌呤溶液剂的含量检测。This paper developed a new formulation of arprinocid,and established a mothod for the determination of arprinocid solution by using high performance liquid chromatography（HPLC）. These results contributed to provide a reference for further application of arprinocid solution. Orthogonal designing method was used to filter out solutions optimal formula,which was based on univariate tests. The best combination of the solution was 40% solvent and 50% co-solvent and 0. 2% antioxidant,and pH value was approximately 3. 0. The content of the solution was determined by HPLC. An C18column（4. 6 mm×250 mm,5. 0 μm） was used,and the proportion of acetonitrice and water which was added with 0. 1% phosphoric and 0. 1% triethanolamine was 18 ∶82 by the mobile phase. Flow rate was 1. 0 mL·min-1,and the column temperature was 30 ℃,and the detection wavelength was 261 nm,with injection volume of 10 μL. Acetic acid was heated to about 40 ℃,then added the dissolved tartaric acid and polyethylene glycol 400,and then filtratted and packed in 100 mL brown glass bottles after being added arprinocid until dissolved. Blank accessories was taken as a blank control,and pipetted for the appropriate amount arprinocid solution,diluted with methanol,with filterring by 0. 45 μm membrane,then injected to detection. Accessories interference test results showed that arpronocid was undisturbed in the peak position. And specificity test revealed that solutions could be separated from degradation products. The linear range of the calibration curve for arprinocid was 50-100 μg·mL-1（R2= 0. 999 3,n = 5）,taking concentration（x） as the abscissa and peak area（y） for the vertical axis linear regression,and regression equation showed y = 34 772x ＋14 371. Pipette exactly 1 mL of arprinocid solution to 100 mL volumetric flask,dissolve it in methanol to the mark,and then place the solution 1 mL to 10 mL volumetric flask with methanol,finally injecte six times continuously. The relative standard deviation（RSD） of precision was

关 键 词：氟腺嘌呤 溶液剂 正交试验 HPLC 测定 

分 类 号：S859.79[农业科学—临床兽医学]