亲水性色谱柱高效液相色谱法测定米面及制品中的二氧化硫脲
目的 建立测定米面及制品中二氧化硫脲的亲水性色谱柱高效液相色谱(high performance liquid chromatography, HPLC)检测方法。方法 样品中的二氧化硫脲经0.5%乙酸提取液在冰浴中超声提取10 min, 10000 r/min离心3 min后取上清液过0.22 μm水相微孔滤膜待测。对10.00 mg/L的二氧化硫脲标准溶液色谱峰进行光谱扫描, 确定二氧化硫脲的最大吸收波长为272 nm。采用Waters XBridge BEH HILIC(150 mm× 4.6 mm, 3.5 μm)色谱柱进行分离, 以纯水:乙腈=20:80(V:V)为流动相, 外标法定量。结果 二氧化硫脲在0~ 50 mg/L范围内, 二氧化硫脲的浓度与色谱峰面积的大小成正比例线性关系。线性方程为Y=1.3701X?0.4482, 相关系数为0.9999。方法检出限为2.00 mg/kg。在方法检出限、2倍方法检出限、10倍方法检出限3个水平进行加标回收实验与精密度实验, 回收率分别为93.0%、95.0%、96.4%, 相对标准偏差分别为5.2%、4.1%、2.5%。结论 该方法准确度与精密度符合GB/T 27404-2008《实验室质量控制规范食品理化检测》的相应技术要求, 方法准确稳定可靠, 满足米面及制品中二氧化硫脲的测定。
Objective To establish a method for the determination of sulfur dioxide in rice, flour and their products by high performance liquid chromatography (HPLC) with urea hydrophilic chromatography column. Methods The thiourea dioxide in the sample was ultrasonically extracted in an ice bath for 10 min with 0.5% acetic acid, centrifuged at 10000 r/min for 3 min, and the supernatant was passed through a 0.22 μm aqueous microporous membrane for testing. A spectral scan of the 10.00 mg/L thiourea standard solution peak was performed to determine the maximum absorption wavelength of thiourea dioxide at 272 nm. Waters XBridge BEH HILIC (150 mm×4.6 mm,3.5 μm) column was used for the separation. Pure water: acetonitrile=20:80(V:V) was used as the mobile phase and external standard method was used for quantification. Results The results showed that in the range of 0-50 mg/L, the concentration of thiourea dioxide was proportional to the size of the chromatographic peak area. The linear equation was Y=1.3701X?0.4482. The correlation coefficient was 0.9999. The limit of detection was 2.00 mg/kg. The standard recovery experiment and precision experiment were carried out at 3 levels with 1, 2 and 10 times of limit of detection, and the recovery rates were 93.0%, 95.0% and 96.4%, respectively. The relative standard deviations were 5.2%, 4.1% and 2.5%, respectively. Conclusion The accuracy and precision of this method conforms to the technical requirements of GB/T 27404-2008 Laboratory quality control standard for food physical and chemical testing. The method is accurate and reliable, which can satisfy the determination of thiourea dioxide in rice, flour and their products.
标题：亲水性色谱柱高效液相色谱法测定米面及制品中的二氧化硫脲
英文标题：Determination of thiourea dioxide in rice, flour and their products by hydrophilic chromatographic column high performance liquid chromatography
作者：
彭名军 广州市食品检验所
宋安华 广州市食品检验所
刘冬豪 广州市食品检验所
黄秋婷 广州市食品检验所
漆亚乔 广州市食品检验所
黄儒强 华南师范大学
中文关键词:二氧化硫脲,亲水性色谱柱,高效液相色谱法,米面制品,
英文关键词:thiourea dioxide,hydrophilic chromatographic column,high performance liquid chromatography,rice, flour and their products,
发表日期：2018-05-07
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