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

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

Key words:  High performance liquid chromatography method  PDAD  Ceftiofur Crystalline Free Acid Injection  Ceftiofur

摘要:

本研究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 UPLCTM C8色谱柱（2.1mm×100mm,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：0.35mL/min；进样量：1μL；检测波长为292nm。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（R2>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。

Abstract:

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 (2.1mm x 100mm,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. 35mL/min, the injection volume is 1μL, and the wavelength is 292nm. 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 4~200μg/mL of ceftiofur, the linear relationship is good (R2>0.9998); The limit of detection is 2μg/mL(S/N>3), and the limit of quantitation is 4μg/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.