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目的超声萃取结合超高效液相色谱(UPLC)技术,建立了米粉中二氧化硫脲的测定方法。方法米粉样品用60%乙腈水(v/v)提取,经离心、过滤后,氨基柱为分析柱进行分离,乙腈和水为流动相等度洗脱,二极管阵列检测器检测,以保留时间和紫外吸收光谱图定性,外标法定量。结果二氧化硫脲在2.0~100.0 mg/L浓度范围内线性关系良好,相关系数为0.9999;方法检出限(S/N=3)为4.0 mg/kg;添加水平为16.0、32.0和160.0mg/kg时,待测物的平均回收率分别为93.5%、107.0%和99.7%,相对标准偏差(RSD,n=6)分别为2.6%、5.2%和7.5%。结论本方法前处理简单、快速、准确,适用于米粉中二氧化硫脲的测定。
Objective To establish a method for the determination of thiourea dioxide in rice flour by ultrasonication combined with ultra-high performance liquid chromatography (UPLC). Methods The samples of rice flour were extracted with 60% acetonitrile water (v / v). After centrifugation and filtration, the amino column was separated on the analytical column. The mobile phase consisted of acetonitrile and water eluted with equal mobility. The diode array detector was used to detect the retention time and UV Absorption spectrogram qualitative, external standard method. Results The concentration of thiourea dioxide was good in the range of 2.0-100.0 mg / L, with a correlation coefficient of 0.9999. The detection limit (S / N = 3) was 4.0 mg / kg and the levels were 16.0, 3.02 and 160.0 mg / kg , The average recoveries of the analytes were 93.5%, 107.0% and 99.7%, respectively. The relative standard deviations (RSDs, n = 6) were 2.6%, 5.2% and 7.5%, respectively. Conclusion The pretreatment method is simple, rapid and accurate and is suitable for the determination of thiourea dioxide in rice flour.