超高效液相色谱法测定头孢噻呋晶体注射液中头孢噻呋含量  

Determination of Ceftiofur in Ceftiofur Crystalline Free Acid Injection by UPLC

作　　者：魏秀丽 常雪 王艳芬 杨志昆 冯言言 张传津 徐恩民 李有志 WEI Xiu-li;CHANG Xue;WANG Yan-fen;YANG Zhi-kun;FENG Yan-yan;ZHANG Chuan-jin;XU En-min;LI You-zhi(Institute of Veterinary Drug Quality Inspection of Shandong Province,Shandong Provincial Key Laboratory of Quality Safety Monitoring andRisk Assessment for Animal Products,China Shandong Engineering Laboratory for Drug Resistance Monitoring andPrecise Drug Use of Animal Origin Bacteria,Jinan 250022,China;Qilu Animal Health Products Co.,Ltd,Jinan 250100,China)

机构地区：[1]山东省兽药质量检验所,山东省畜产品质量安全监测与风险评估重点实验室,动物源细菌耐药性监测与精准化用药山东省工程实验室,济南250022 [2]齐鲁动物保健品有限公司,济南250100

出　　处：《中国兽药杂志》2020年第10期10-15,共6页Chinese Journal of Veterinary Drug

基　　金：2015年国家科技支撑计划“兽药安全与质量评价技术研究与应用”(BAD11B03-01)。

摘　　要：建立超高效液相色谱-光电二极管阵列法(UPLC-PDA)测定头孢噻呋晶体注射液中主成分头孢噻呋的含量。采用反相超高效液相色谱法对头孢噻呋进行色谱分离和快速定量测定。以ACQUITY UPLCTMC8色谱柱(2.1 mm×100 mm,1.7μm)为分离柱,柱温:35℃;以乙腈-水(0.1%甲酸)进行梯度洗脱;流速:0.35 mL/min;进样量:1μL;检测波长为292 nm。通过光谱图、保留时间和峰面积参数对头孢噻呋进行定性、定量检测。头孢噻呋在4~200μg/mL的范围内线性关系良好(R^2>0.9998);方法检测限为2μg/mL、定量限为4μg/mL,完全满足检测需求。该方法色谱分离较好,分析速度较快,前处理简单,适用于头孢噻呋晶体注射液中主成分头孢噻呋含量的检测。This study aims to establish a high performance liquid chromatography(UPLC-PDA) test method for the determination of ceftiofur in ceftiofur crystalline free acid injection. UPLC was used to isolate and quantitatively determine ceftiofur. ACQUITY UPLCTM C8 chromatographic column(2.1 mm x 100 mm,1.7 μm) was used as the separation column, Column temperature 35 ℃;Gradient elution was performed with acetonitrile-water(0.1% formic acid) solution as mobile phase;The flow rate is 0. 35 mL/min, the injection volume is 1 μL, and the wavelength is 292 nm. In this paper, the quantitative and qualitative determination of ceftiofur was carried out by spectrogram, retention time and peak area parameters. In the range of 4~200 μg/mL of ceftiofur, the linear relationship is good(R^2>0.9998);The limit of detection is 2 μg/mL(S/N>3), and the limit of quantitation is 4 μg/mL(S/N>10), which fully meet the requirements. The test method is suitable for the qualitative and quantitative determination of ceftiofur in ceftiofur crystalline free acid injection for its good separation, quick analysis and easy sample treatment performance.

关 键 词：超高效液相色谱法 光电二极管阵列检测器 头孢噻呋晶体注射液 头孢噻呋 

分 类 号：S859.795[农业科学—临床兽医学]