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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 |
| 阅读数： | 374 次 |
| 本月下载数： | 11 次 |
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