不同分析技术测定调味品中3-氯-1,2-丙二醇的应用研究

Determining 3-chloro-1,2-propandiol in condiments by different methods

目的比较国际公认的稳定性同位素稀释质谱技术(内标法)和外标法,对检测调味品中3 -氯-1, 2 -丙二醇(3-MCPD)的差异;和硅藻土柱层析分离技术与SPE小柱分离技术,在萃取净化调味品中3 -MCPD的效果。方法应用气相色谱-质谱测试技术,选择离子储存(SIS)模式。结果①在检出3-MCPD的12份样品中,内标法的总体测定结果高于外标法[0 172±0 122(内标法)、0 122±0 062(外标法) ],但结果无显著性差异(P>0 05)。②硅藻土层析柱萃取净化调味品中3-MCPD,洗脱液的色素和杂质含量均小于SPE小柱。结论硅藻土柱层析分离调味品中3-MCPD的效果优于SPE小柱,稳定性同位素内标法的应用,进一步提高了方法的精密度和准确度。

Objective:To compare the results of determining 3-chloro-1,2-propandiol(3-MCPD) in condiments by applying deuterium-labeled isotope internal standard(IS) with those by applying exterior standard(ES), and to compare the effects of the solid-phase extraction with Extrelut^TM NT with the solid-phase extraction(SPE). Methods:The capillary gas chromatography-ion trap mass spectrometry was used by selecting the storage (SIS) mode.Results:①3-MCPD was found in 12 samples. The value determined by IS(0.172±0.122) was higher than ES(0.122±0.062)(P>0.05). ②The pigments and the impurities extracted by Extrelut^TM NT were less than those extracted by SPE.Conclusion:The samples which were spiked with deuterium-labeled isotope internal standard and extracted by solid-phase extraction with Extrelut^TM NT were developed with better accurateness and precision. [