HPLC-APCI-MS法快速测定面包中联二脲的含量

Determination of hydrazodicarbonamide in bread by high performance liquid chromatography in tandem atmospheric pressure chemical ionization source mass spectrometry

为快速检测面包中的联二脲(HDC)含量,建立高效液相色谱串联大气压化学电离源质谱(HPLC-APCI-MS)法快速测定面包中联二脲含量的方法。采用80℃水作为提取剂,正己烷萃取除去样品杂质,净化后的样品采用Xbridge BEH Prep OBD Amide色谱柱进行分离,以体积比3:7的水—乙腈溶液为流动相,流速0.6 mL/min,进行梯度洗脱,大气压化学电离源(APCI)正离子模式电离,多反应监测模式检测,外标法定量,采用添加回收法进行测定。结果表明,该测定方法适用线性范围为0.2~10.0 mg/L,相关系数为99.5%~99.9%。室内平均回收率为82%~110%,实验室内精密度<10.3%,能够满足一般分析方法的要求。该方法操作简便、快速、灵敏度高,适合面包中联二脲含量的测定。

A method of determining the content of hydrazodicar bonamide （ HDC ） in bread by high performance liquid chromatography in tandem atmospheric pressure chemical ionization source mass spectrometry （HPI.C-APCI-MS） was established. Using 80℃ water as extractant, N hexane extraction was used to remove sample impurities. And then the samples purified were separated by using Xbridge BEH Prep OBD Amide column. The gradient elution was performed by using water ： acetonitrile （3 ： 7） （v/v）, with the flow velocity 0.6 mL/min. The ionization were achieved by using AP- CI source positive ion mode with MRM scan mode. The internal standard calibration curves were used for quantitative. The method of adding-recovery were used to test. The results showed good linearity in the range of 0.2-10.0 mg/L, and the correlation coefficient was 99.5%-99.9%. The indoor average recovery was between 82%-110% and the precision of the laboratory was less than 10.3G, which could satisfy the general requirement of analysis method. Mo- reover, the method is simple, rapid and sensitive, which is suitable for the determination of HDC in bread.