超高效液相色谱-串联质谱法测定血浆中烷基间苯二酚

目的:建立超高效液相色谱-串联质谱法测定血浆中2种全麦食品生物标志物烷基间苯二酚(ARs)的方法。方法:血浆加入内标,经丙酮提取,离心取上清液过滤,滤液吹干异丙醇定容,使用实心核色谱柱(2.1mm×100mm,1.6μm)为分离柱,以异丙醇∶乙腈=30∶70为流动相,等度洗脱,质谱采用电喷雾负离子模式,多反应监测模式进行检测,用内标法定量。结果:2种ARs在2~200ng/mL浓度范围内线性良好,r 2>0.9980。方法检出限为0.1ng/mL,定量限为0.3ng/mL,加标回收率为88.2%~110%,相对标准偏差为2.48%~13.2%(n=6)。结论:该方法快速准确、灵敏度高、前处理简单,能够有效测定血浆中2种ARs的含量。

Determinnation of Alkylresorcinols in Plasma by UPLC-MS/MS

Objective To establish a method for the determination of 2 alkylresorcinols as biomarkers of whole-grain wheat foods by ultra high performance liquid chromatography-tandem triple quadrupole mass spectrometry(UPLC-MS/MS).Method Internal standard was added in plasma,the ARs was extracted by acetone,the extraction was filtrated and dried under nitrogen,and then dissolved in isopropanol for analysis.The analysis was performed on a cortecs column(2.1mm×100mm,1.6μm)and isocratic elution using isopropanol∶acetonitrile=30∶70 as the mobile phase.The samples were determined by mass spectrometry in the negative ion mode with the multiple reaction monitoring mode,quantified by the internal standard method.Result Totally 2 alkylresorcinols had good linearity in the concentration range of 2~200 ng/mL,r 2>0.9980.The limits of detection for 2 alkylresorcinols was 0.1ng/mL,the limits of quantification was 0.3ng/mL.Re coveries at 3 different levels were in ranges of 88.2%~110%,and the relative standard deviations were in ranges of 2.48%~13.2%(n=6).Conclusion This method is accurate and sensitive,the preparation is simple and rapid,which can be used for determination of 2 alkylresorcinols in plasma effectively.