超高效液相色谱法测定米粉中的二氧化硫脲

Determination of thiourea dioxide in rice flour by ultra-high performance liquid chromatography

中文关键词:  二氧化硫脲  米粉  超声萃取  超高效液相色谱法

英文关键词:thiourea dioxide  rice flour  ultrasonic extraction  ultra-high performance liquid chromatography

中文摘要:

      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160.0 mg/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。

英文摘要:

      Objective A new method was established to determine thiourea dioxide(TDO) in rice flour samples by ultrasonic extraction combined with ultra-high performance liquid chromatography(UPLC). Methods In the study, the rice flour samples were extracted with 30% acetonitrile water(v/v), then the extracts were centrifuged, filtrated, and analyzed by Amide column, employing acetonitrile and water as the mobile phases under the condition of Isocratic elution．The thiourea dioxide were qualitatively determined by retention times, and confirmed by ultraviolet spectra．The external standard method was applied for the quantification. Results In the concentration of 2.0~100.0 mg/L, the target analyte showed that a correlation coefficient was 0.9999, and a method detection limit(LOD) was 4.0 mg/kg (S/N=3). The feasibility of this method was demonstrated by identifying TDO in rice flour samples that exhibited spiked recoveries were 93.5%, 107.0% and 99.7% (n=6), and the precision were 2.6%, 5.2% and 7.5% (n=6). Conclusion The presented method is simple, fast, and accurate for the determination of TDO in rice flour samples.