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
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篇名: 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
TITLE:
摘要: 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2 μL;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/mL(r=0.999 4);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。
ABSTRACT: 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 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 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/mL(r=0.999 4); 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.
期刊: 2017年第28卷第9期
作者: 罗达龙,王华
AUTHORS: LUO Dalong,WANG Hua
关键字: 超高效液相色谱-串联质谱法;固相萃取;桔霉素;残留量;脂必妥片
KEYWORDS: UPLC-MS/MS; Solid phase extraction; Citrinin;Residual; Zhibituo tablets
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