摘要:
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°C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 (HPLC-APCI-MS) was established.Using 80 °C 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 10.3%,which could satisfy the general requirement of analysis method.Moreover,the method is simple,rapid and sensitive,which is suitable for the determination of HDC in bread.