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目的采用液相色谱-电喷雾离子阱质谱联用法(HPLC/MS/MS),以保留时间、结构和分子量信息为指标测定抗风湿、镇痛类中药制剂中可能添加的糖皮质激素类化学药醋酸泼尼松及泼尼松。方法建立HPLC/MS/MS方法,液相色谱:色谱柱为AgilentC18柱,以0.01mol/L甲酸铵溶液(甲酸调节pH值至4.0)-甲醇(30:70)为流动相,流速0.4mL/min,柱温30℃,检测波长270nm;质谱:电喷雾离子源正离子检测方式(ESI+),m/z范围50～1000,离子源喷射电压5KV,雾化电压40psi,干燥气温度350℃,干燥气(N2)流速10L/min,毛细管电压15V。结果通过与对照品峰的保留时间及一级、二级质谱图谱比较,确定样品中是否添加了化学药。应用该法在供试品溶液中检出了醋酸泼尼松。结论该方法选择性强,可用于鉴别中药制剂中非法添加糖皮质激素类化学药醋酸泼尼松及泼尼松。
Objective To determine the possible glucocorticoids in the preparation of anti-rheumatic and analgesic preparations using liquid chromatography-electrospray ion trap mass spectrometry (HPLC/MS/MS) with retention time, structure and molecular weight information as indicators. Prednisone acetate and prednisone. METHODS HPLC/MS/MS method was established. The liquid chromatography was performed on an Agilent C18 column using a 0.01 mol/L ammonium formate solution (formic acid to adjust the pH to 4.0) and methanol (30:70) as the mobile phase. The flow rate was 0.4 mL/liter. Min, column temperature 30°C, detection wavelength 270nm; mass spectrometry: electrospray ionization source positive ion detection method (ESI+), m/z range 50 to 1000, ion source injection voltage 5KV, atomization voltage 40 psi, drying gas temperature 350°C, Dry gas (N2) flow rate 10 L/min, capillary voltage 15V. The results were compared with the retention time of the reference peak and the primary and secondary mass spectra to determine if the chemical was added to the sample. This method was used to detect prednisone acetate in the test solution. Conclusion The method is highly selective and can be used to identify prednisone acetate and prednisone acetate, which are illegally added to glucocorticoids.