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目的:建立液相色谱串联质谱法和高效液相色谱-示差折光法测定注射用磷霉素钠中的磷霉素钠二醇物含量,并与现行中国药典方法比较,提高对药品的质量控制。方法:液相色谱串联质谱法采用Promosil CN(250 mm×4.6 mm,5μm)色谱柱,流动相为5 mmol.L-1醋酸铵-甲醇(82∶18),采用(-)ESI电离源,多反应监测(MRM)扫描方式,用于定量分析的离子分别为m/z 154.9→80.9(磷霉素二醇物)和m/z 120.9→77.1(内标苯甲酸)。高效液相色谱-示差折光法采用Agilent Zorb-ax NH2(250 mm×4.6 mm,5μm)色谱柱,流动相为10.89 g.L-1磷酸二氢钾溶液,流速为1.0 mL.min-1;柱温36℃;检测器温度为35℃。结果:采用液相色谱串联质谱法,二醇物在22.46～359.4 ng.mL-1范围内线性关系良好,定量限为4.492 ng.mL-1,每一样品的分析时间为5 min。采用高效液相色谱-示差折光法,二醇物在0.104～5.205 mg.mL-1浓度范围内线性关系良好,精密度为0.7%,重复性良好。结论:本研究2种方法专属性高、简便、可靠,可用于注射用磷霉素钠的质量研究和质量控制。
OBJECTIVE: To establish a liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) and high performance liquid chromatography-refractive index method for the determination of fosfomycin sodium diols in fosfomycin sodium for injection and to improve the quality control of the drugs compared with the current Chinese pharmacopoeia . METHODS: Liquid chromatography tandem mass spectrometry was performed on a Promosil CN (250 mm × 4.6 mm, 5 μm) column with a mobile phase of 5 mmol·L-1 ammonium acetate-methanol (82:18) Multiple reaction monitoring (MRM) scanning mode for the quantitative analysis of ions were m / z 154.9 → 80.9 (fosfomycin diol) and m / z 120.9 → 77.1 (internal standard benzoic acid). High performance liquid chromatography with differential refractive index was performed on an Agilent Zorb-ax NH2 (250 mm × 4.6 mm, 5 μm) column with a mobile phase of 10.89 gL-1 potassium dihydrogen phosphate at a flow rate of 1.0 mL.min-1. The column temperature 36 ° C; detector temperature 35 ° C. Results: The liquid chromatography tandem mass spectrometry (LC-MS / MS) showed a good linearity of the range of 22.46-359.4 ng.mL-1 with a limit of quantification of 4.492 ng.mL-1. The analysis time of each sample was 5 min. High performance liquid chromatography - differential refractive index method, diol in the concentration range of 0.104 ~ 5.205 mg.mL-1 good linearity, precision of 0.7%, good reproducibility. Conclusion: The two methods in this study are highly specific, simple and reliable and can be used for the quality control and quality control of fosfomycin sodium for injection.