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本实验建立了一种灵敏且专属的HPLC-DAD测定家兔关节液中头孢唑林钠的方法。用乙腈沉淀关节液中的蛋白质,安替比林作为内标。样品在戴安U3000高效液相色谱仪上操作,并用菲罗门Luna C18(150 mm×4.60 mm,5μm,100 A)柱分离,流动相为0.1%甲酸水和乙腈,流速为1 mL/min,检测波长为272 nm,柱温为25 oC。在1.0–100.0μg/mL范围内,头孢唑林钠和内标安替比林的峰面积比值与浓度线性关系良好(r 2=0.9999),最低检测限为(LOD,S/N=3)为0.07μg/mL,最低定量限(LOD,S/N=10)为0.22μg/mL。头孢唑林钠回收率(低、中、高浓度)分别为124.6%、117.8%、100.6%(RSD%=1.9%,4.0%,1.1%,n=5)。日内和日间精密度在0.5%–2.7%。本实验建立的家兔关节液中头孢唑林钠HPLC-DAD分析方法简便、灵敏且可靠。此方法可以应用于家兔关节液中头孢唑林钠的测定。
This experiment established a sensitive and exclusive HPLC-DAD method for the determination of cefazolin sodium in rabbit joint fluid. Acetonitrile was used to precipitate the protein in the synovial fluid, with antipyrine as the internal standard. The samples were run on a Diane U3000 high performance liquid chromatograph and separated on a Phenomenex Luna C18 (150 mm × 4.60 mm, 5 μm, 100 A) column with a mobile phase of 0.1% formic acid in water and acetonitrile at a flow rate of 1 mL / min , The detection wavelength is 272 nm, the column temperature is 25 oC. In the range of 1.0-100.0μg / mL, the peak area ratio of cefazolin sodium and the internal standard antipyrine has a good linear relationship (r 2 = 0.9999) and the minimum detection limit (LOD, S / N = 3) Was 0.07 μg / mL and the lowest limit of quantification (LOD, S / N = 10) was 0.22 μg / mL. The recoveries of cefazolin sodium (low, medium and high) were 124.6%, 117.8% and 100.6%, respectively (RSD% = 1.9%, 4.0%, 1.1%, n = 5). Intra- and inter-day precision is between 0.5% -2.7%. The HPLC-DAD method for the determination of cefazolin sodium in rabbit's synovial fluid established in this experiment is simple, sensitive and reliable. This method can be applied to the determination of cefazolin sodium in rabbit synovial fluid.