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

Determination of Residual Citrinin in Zhibituo Tablets by Solid Phase Extraction-UPLC-MS/MS

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 C_(18),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 m L/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3 500 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/m L(r=0.999 4);定量限和检测限分别为0.05、0.01 ng/m L;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。

OBJECTIVE：To determine residual citrinin in Zhibituo tablet by solid phase extraction-UPLC-MS/MS. METHODS：The sample was processed preliminary by solid extraction. The determination was performed on Zorbax Eclipse Plus C18 column with mobile phase consisting of water（0.1% formic acid）-acetonitrile（70 ∶ 30,V/V,gradient elution） at the follow rate of0.30 m L/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 3 500 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/m L（r=0.999 4）;the limits of quantitation and detection were 0.05 and 0.01 ng/m L. RSDs of precision,stability and repeatability tests were all lower than2.0%;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.