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目的:建立SPE-LC-MS/MS法测定重组人粒细胞刺激因子注射液中氨苄青霉素残留。方法:选择阿莫西林为内标,样品经过HLB固相萃取小柱净化,浓缩,有效地去除杂质。采用Agilent Eclipse XDB-C18(4.6 mm×150 mm,5μm)色谱柱,以乙腈-水(甲酸调pH 3.1)为流动相进行梯度洗脱。采用电喷雾离子源(ESI),正离子模式,多反应监测(MRM)。氨苄青霉素,内标监测离子对的m/z分别为350.0/106.1,350.0/192.0和366.0/114.0,366.0/208.0。结果:氨苄青霉素浓度在0.0442～3.5362μg.L-1范围内线性关系良好(r=0.9995),最低定量限为0.0442μg.L-1,方法回收率在101.1%～106.7%之间,批内,批间RSD分别小于5.8%及7.3%。结论:本方法准确可靠,重复性好,灵敏度高,适用于重组人粒细胞刺激因子注射液中氨苄青霉素残留检测。
OBJECTIVE: To establish a method for the determination of ampicillin residues in recombinant human granulocyte-stimulating factor injection by SPE-LC-MS / MS. Methods: Amoxicillin was selected as internal standard. The sample was purified by HLB solid phase extraction cartridge and concentrated to effectively remove impurities. The column was eluted with an Agilent Eclipse XDB-C18 (4.6 mm × 150 mm, 5 μm) column using a mobile phase of acetonitrile-water (pH 3.1 for formic acid). Electrospray ionization (ESI), positive ion mode, multiple reaction monitoring (MRM) were used. Ampicillin, internal standard ion pairs monitored m / z 350.0 / 106.1, 350.0 / 192.0 and 366.0 / 114.0, 366.0 / 208.0, respectively. Results: The linearity of ampicillin in the range of 0.0442 ~ 3.5362μg.L-1 was good (r = 0.9995), the lowest limit of quantification was 0.0442μg.L-1, and the recoveries were between 101.1% and 106.7% Inter-lot RSD was less than 5.8% and 7.3% respectively. Conclusion: The method is accurate, reliable, reproducible and sensitive. It is suitable for the detection of ampicillin residues in recombinant human granulocyte-stimulating factor injection.