OBJECTIVE:To determine residual citrinin in Zhibituo tablet by solid phase extraction-UPLC-MS/MS. METH-ODS:The sample was processed preliminary by solid extraction. The determination was performed on Zorbax Eclipse Plus C18 col-umn with mobile phase consisting of water (0.1% formic acid)-acetonitrile (70:30,V/V,gradient elution) at the follow rate of 0.30 mL/min. The column temperature was 40 ℃,and analysis time was 7 min,the sample size was 2 μL. Ionization mode was positive ion mode. The ion source temperature was 150 ℃,drying gas velocity was 15 L/min,sheath gas temperature was 350 ℃, sheath gas flow rate was 12 L/min,capillary voltage was 3500 V,atomization device pressure was 40 psi,atomization voltage was 0 V. The acquisition mode was MRM mode. RESULTS:The linear range of citrinin was 0.1-20 ng/mL(r=0.9994);the limits of quantitation and detection were 0.05 and 0.01 ng/mL. RSDs of precision,stability and repeatability tests were all lower than 2.0%;recoveries were 98.868%-103.160%(RSD=1.5%,n=6). CONCLUSIONS:The method is rapid,sensitive,accurate and suitable for the determination of residual citrinin in Zhibituo tablet.%目的:采用固相萃取-超高效液相色谱-串联质谱法测定脂必妥片中桔霉素的残留量.方法:采用固相萃取法进行前处理,色谱柱为Zorbax Eclipse Plus C18,流动相为水(加0.1%甲酸)-乙腈(70:30,V/V)(梯度洗脱),流速为0.30 mL/min,柱温为40℃,分析时间为7 min,进样量为2μL;离子化模式为正离子模式,离子源温度为150℃,干燥气流速为15 L/min,鞘气温度为350℃,鞘气流速为12 L/min,毛细管电压为3500 V,雾化器压力为40 psi,喷雾电压为0 V,工作模式为多反应监测模式.结果:桔霉素检测质量浓度线性范围为0.1~20 ng/mL(r=0.9994);定量限和检测限分别为0.05、0.01 ng/mL;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率为98.868%~103.160%(RSD=1.5%,n=6).结论:该方法简便快速、灵敏、结果准确,适用于脂必妥片中桔霉素的残留量测定.
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