HPLC法测定米卡芬净起始物料FR179642的含量

摘要

Objective To establish the method for content determination of FR179642 that is the Starting Material for synthesizing Micafungin.Methods HPLC method was adopted. The determination was performed on Thermo UltiMate 3000 YMC C18(150×4.6 mm,120 A,3μm). The moving phase A and B were 0.01%TFA-water and 0.01%TFA-methanol, respectively. The process of gradient elution was at the flow rate of 0.5 mL/min as: 0~20 min, 1% moving phase B; 20~30 min, 1~20% moving phase B; 30~35 min, 20~60% moving phase B; 35~36 min, 60% moving phase B. The detection wavelength was set at 225 nm and the sample size was 10μL with temperature of 50℃.Results The equation of linear regression wasY=1 343 7522.790 7X-92 432.259 2(r=0.999 9) with the linear range of 0.273 8~0.912 7 mg/mL and an total average recovery of 99.97%(RSD=0.46%,n=9).Conclusion The method is simple, rapid, and reliable, and suitable for the quality control of Micafungin Starting Material FR179642.%目的：建立测定合成米卡芬净起始物料FR179642含量的方法。方法采用高效液相色谱法（HPLC），色谱柱为Thermo UltiMate 3000 YMC C18（150×4.6 mm，120 A，3μm）；流动相A：0.01%三氟乙酸-水；流动相B：0.01%三氟乙酸-甲醇；梯度洗脱：0～20 min，1%流动相B；20～30 min，1%～20%流动相B；30～35 min，20%～60%流动相B；35～36 min，60%流动相B；流速：0.5 mL/min；检测波长：225 nm；进样量：10μL；柱温：50℃。结果米卡芬净起始物料FR179642的线性回归方程Y＝13437522.7907X-92432.2592（r＝0.9999），线性范围0.2738～0.9127 mg/mL，总平均回收率99.97%（RSD＝0.46%，n＝9）。结论HPLC含量测定方法简便、快捷、可靠，可用于米卡芬净起始物料FR179642的质量控制。