LC-MS/MS测定碘海醇及其注射剂中有关物质的研究

 目的 建立液相色谱-串联质谱联用方法，对碘海醇及其注射剂中两种有关物质进行分离和测定。方法 色谱柱：Agilent C₁₈分析柱（4.6 mm×150 mm，3.5 μm），流动相为0.05%的甲酸水溶液(A)和乙腈(B)，进行梯度洗脱，流速0.25 mL·min-1，柱温为30 ℃，采用ESI离子化-串联质谱选择离子监测（SRM）正离子模式检测，喷雾电压：3 500 V，鞘气流速：30 L·min-1，辅助气流速：5 L·min-1，毛细管温度：325 ℃，离子选择通道分别为m/z 747.8/528.9（有关物质A）、m/z 705.8/614.9（有关物质B）和m/z 328.2/237.3（内标）。结果 该方法中有关物质A、有关物质B分别在0.281 7～11.27 mg·L-1（r=0.999 4）和27.00～1 080 μg·L-1（r=0.996 3）内线性关系良好，有关物质A、有关物质B在高、中、低3个浓度的平均回收率分别为103.2%（RSD为4.4%）、105.4%（RSD为7.8%）。结论 该方法可同时测定碘海醇及其注射剂中的两种有关物质。

Simultaneous Determination of Two Related Compounds in Iohexol and Its Injection by LC-MS/MS

OBJECTIVE A LC-MS/MS method for the determination of two related compounds in iohexol and its injection was established firstly. METHODS An Agilent C₁₈ (4.6 mm×150 mm，3.5 μm) column was used with the mobile phase of water (0.05% formic acid， A) and acetonitrile(B)， the flow rate was 0.25 mL·min-1， the column temperature was 30 ℃. Sample was analyzed by electrospray ionization applying selected reaction monitoring (SRM) scan type. The spray voltage was set at 3 500 V， transfer capillary temperature was at 325 ℃， the pressures of sheath gas and auxiliary gas (nitrogen) were at 30 and 5 L·min-1. The selected ions for mass monitoring were m/z 747.8/528.9 (related compound A)， m/z 705.8/614.9 (related compound B) and m/z 328.2/237.3 (IS). RESULTS The linear ranges of related compound A and B were 0.281 7-11.27 mg·L-1（r=0.999 4）and 27.00～108 0 μg·L-1 (r=0.996 3)， respectively. The average recoveries of related compound A and B at three levels were 103.2% (RSD 4.4%) and 105.4% (RSD 7.9%)， respectively. CONCLUSION The established LC-MS/MS method can measure two related compounds in iohexol and its injection simultaneously and accurately.