摘要
为了验证检测替米考星纳米内服混饮剂中替米考星含量的高效液相色谱法(HPLC法)的方法学可靠性,试验用乙腈水(1∶1)200倍稀释替米考星纳米内服混饮剂,水浴10min,12000r/min离心30min,用磷酸稀释液稀释1000倍;用AgilentSBC18(250mm×4.6mm×5μm)色谱柱,以865mL超纯水、55mL乙腈、55mL四氢呋喃、25mL磷酸二丁胺缓冲液为流动相,流速1.0mL/min,检测波长280nm,用HPLC法进行含量测定的方法学验证。结果表明:建立的替米考星纳米内服混饮剂含量测定的HPLC法标准曲线方程为:A=7808.8C+2314.6,R^2=0.9999,替米考星在5~100μg/mL浓度范围内线性关系良好;平均回收率为(100.03±0.52)%,RSD为0.88%;日内稳定性的RSD为1.29%,日间稳定性的RSD为0.26%;样品平均含量为4.81%。表明所建立的方法专属性强、简便、可行,可用于替米考星纳米内服混饮剂中替米考星含量的测定。
In order to verify the methodological reliability of HPLC method for the determination of timicorcine content in timicorcine nano-oral mixed potions;The tilmicosin nano-oral mixed potions was diluted 200 times with acetonitrile: water(1∶1) and kept in a water bath for 10 min,and then was centrifuged at 12 000 r /min for 30 min;The supernatant was diluted 1 000 times with phosphoric acid solution. Agilent SB C18 column( 250 mm×4. 6 mm×5 μm) was used;The mobile phase was 865 mL ultra-pure water;55 mL acetonitrile;55 mL tetrahydrofuran;and 25 mL dibutylamine phosphate buffer;The flow rate was 1. 0 mL /min;the detection wavelength was 280 nm;and HPLC was adopted for the methodological verification of content determination;The results showed that the established HPLC calibration curve equation for the content determination of tilmicosin nano-oral mixed potions was: A = 7 808. 8C+2 314. 6,R^2 = 0. 999 9,and timicorcine had a good linear relationship within the concentration range of 5-100 μg /mL;The average recovery rate was( 100. 03±0. 88)%;with the RSD of 0. 88%;the intraday stability RSD of 1. 29%;and the daytime stability RSD of 0. 26%;the average content was 4. 81%. The results suggested that the established method was specific;simple and feasible;and can be used for the content determination of tilmicosin in tilmicosin nano-oral suspension.
作者
李超
赵海旭
周凯翔
王志霞
罗万和
谢书宇
LI Chao;ZHAO Haixu;ZHOU Kaixiang;WANG Zhixia;LUO Wanhe;XIE Shuyu(National Reference Laboratory of Veterinary Drug Residues,Huazhong Agricultural University,Wuhan 430070,China;State Key Laboratory of Agricultural Microbiology,Huazhong Agricultural University,Wuhan 430070,China)
出处
《黑龙江畜牧兽医》
CAS
北大核心
2019年第15期124-127,共4页
Heilongjiang Animal Science And veterinary Medicine
基金
国家重点研发计划专项“新型动物药剂创制与产业化”(2017YFD0501403)
