建立了测定发酵液中喷司他丁含量的反相高效液相色谱-质谱分析方法.采用的色谱条件:色谱柱为Hypersil ODS2柱(250 mm×4.6 mm,5 μm);流动相为甲醇/乙腈/10 mmol/L 乙酸铵(pH 7.6)(2.5/2.5/95,v/v/v),流速为1.0 mL/min;检测波长为280 nm;柱温为40 ℃;进样量为10 μL.喷司他丁在1.0～100 mg/L 范围内有良好的线性关系,相关系数为 0.999 9.该方法精密度好,稳定性高,能简便、快速、准确地测定发酵液中喷司他丁的含量.
A method for the determination of pentostatin in culture broth was established using high performance liquid chromatography-mass spectrometry (HPLC-MS).The chromatographic conditions used were as follows:the analytical column was Hypersil ODS2 (250 mm×4.6 mm,5 μm);the mobile phase was methanol/acetonitrile/10 mmol/L ammonium acetate (pH 7.6) (2.5/2.5/95,v/v/v) with a flow rate of 1.0 mL/min;the detection wavelength was 280 nm;the injection volume was 10 μL;the temperature was 40 ℃.The linear range of the method for pentostatin was 1.0-100 mg/L (r=0.999 9).The method is characterized by simplicity,higher sensitivity and accuracy.
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