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目的建立馅料中二氧化硫脲的超高效液相色谱测定方法。方法用0.05%乙酸水溶液提取,样品提取液经过离心,乙腈稀释过滤膜过滤后,以HILIC色谱柱为分析柱分离,采用超高效液相色谱-二极管阵列检测器(ultra performance liquid chromatography-photo-diode array,UPLC-PDA)检测,以乙腈和水为流动相,梯度洗脱,检测波长为284 nm。采用外标法定量。结果二氧化硫脲的线性范围为0.4~20.0 mg/L,相关系数不小于0.999,空白样品的加标回收的回收率为80.6%~102.2%,相对标准偏差为2.6%~5.0%。结论该方法简便、快速、准确、重现性好,适用于馅料中二氧化硫脲的检测。
Objective To establish a method for the determination of thiourea dioxide in fillings by ultra performance liquid chromatography. The method was extracted with 0.05% acetic acid aqueous solution, the sample extract was centrifuged, diluted with acetonitrile, filtered through a membrane, separated on a HILIC column and analyzed by ultra performance liquid chromatography-diode-array detector array, UPLC-PDA). The mobile phase consisted of acetonitrile and water with a gradient of 284 nm. Using external standard method. Results The linear range of thiourea dioxide was 0.4-20.0 mg / L, the correlation coefficient was no less than 0.999. The spiked recoveries of spiked samples ranged from 80.6% to 102.2% with relative standard deviations from 2.6% to 5.0%. Conclusion The method is simple, rapid, accurate and reproducible. It is suitable for the detection of thiourea dioxide in fillings.