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目的建立超高效液相色谱-质谱联用法(UPLC-MS)对碘佛醇主成分异构体及有关物质同时进行分离检测和结构鉴定。方法采用Waters ACQUITY UPLCTMBEH C8(2.1 mm×100 mm,1.7μm)色谱柱,流动相为乙腈-0.1%甲酸溶液(3∶97),检测波长为254 nm;电喷雾离子源,检测模式为正离子,锥孔电压为80 V。结果碘佛醇4个光学异构体及有关物质分离良好,并且通过了质谱、紫外光谱和液相色谱的确证。碘佛醇、杂质Ⅰ和杂质Ⅱ分别在0.5~52.8、0.2~9.3、0.5~28.4μg·m L-1内呈良好的线性关系(r=0.999 9);检出限分别为0.2、0.08、0.2μg·m L-1。结论该方法简便、灵敏、准确,可用于碘佛醇主成分异构体及有关物质的同时分离检测。
OBJECTIVE To establish a method for the simultaneous determination and identification of ioversol isomers and related substances by UPLC-MS. Methods The mobile phase consisted of acetonitrile-0.1% formic acid solution (3:97) with a detection wavelength of 254 nm on a Waters ACQUITY UPLC TMBEH C8 (2.1 mm × 100 mm, 1.7 μm) column. The electrospray ionization source , Cone voltage is 80 V. Results The four optical isomers of Ioversol and related substances were well separated and confirmed by MS, UV and LC. Ioversol, impurity I and impurity II showed a good linearity (r = 0.999 9) in the range of 0.5-52.8, 0.2-9.3 and 0.5-28.4 μg · m L-1, respectively. The detection limits were 0.2,0.08, 0.2 μg · m L-1. Conclusion The method is simple, sensitive and accurate and can be used for the simultaneous separation and detection of ioversol main isomers and related substances.