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建立了采用高效液相色谱-串联质谱(HPLC-ESI-MS/MS)分析中生菌素(zhongshengmycins)原药中各有效成分(链丝菌素A～F)的方法。原药用去离子水超声辅助提取后经离心过滤,反相离子对高效液相色谱分离,二级质谱检测,标准样品定量离子外标法定量。结果表明:在15.63～500μg/mL质量浓度范围内,中生菌素原药各组分的仪器响应值与进样质量浓度之间呈良好的线性关系,相关系数R2>0.990 5;方法具有较好的精密度和准确度,6次重复进样,其相对标准偏差(RSD)在0.33%～1.96%之间;在0.1、0.5和1μg/mg 3个添加水平下,各组分的回收率在98.2%～101.1%之间。样品实测结果表明:供试原药中链丝菌素D的含量最高,为297.65μg/g;其次是链丝菌素B、C和F,含量分别为247.77、285.64和115.92μg/g;链丝菌素A和E的含量较低,分别为15.63和19.60μg/g。该方法能满足中生菌素原药中各有效成分定性及定量分析的要求。
A method was developed for the determination of each active ingredient (streptozotocin A ~ F) in zhongshengmycins by high performance liquid chromatography-tandem mass spectrometry (HPLC-ESI-MS / MS). The original medical deionized water ultrasound-assisted extraction by centrifugation, reverse phase ion-pair high performance liquid chromatography, secondary mass spectrometry, standard sample quantitative ion external standard method. The results showed that there was a good linear relationship between the instrumental response value and the injection quality concentration of the components of the original strain of meconazole within the concentration range of 15.63 ~ 500μg / mL with the correlation coefficient R2> 0.9905. Good precision and accuracy, with 6 repeated injections, the relative standard deviations (RSDs) ranged from 0.33% to 1.96%. The recoveries of the three components at 0.1, 0.5 and 1 μg / mg Between 98.2% and 101.1%. The results showed that streptozotocin D had the highest content of 297.65μg / g, followed by streptozotocin B, C and F, with the contents of 247.77,285.64 and 115.92μg / g, respectively. The contents of streptozotocin A and E were lower at 15.63 and 19.60 μg / g, respectively. The method can meet the requirements of the qualitative and quantitative analysis of the active ingredients in the original biotin.