UPLC-MS/MS测定葡萄酒中29 种单体酚方法的建立

目的：超高效液相色谱-串联质谱技术建立同时测定葡萄酒中29 种单体酚的快速检测方法。方法：样品经过酸化甲醇稀释高速离心后取上清液进样分析，使用ACQUITY UPLC? BEH C18色谱柱洗脱分离，流动相为0.1%甲酸-乙腈和0.1%甲酸，电喷雾离子源，负离子模式，多反应监测；离子源温度500 ℃；电喷雾电压－4 500 V；气帘气压力40 psi；碰撞气：Medium；雾化气压力60 psi；辅助加热气压力50 psi，分析时间17 min。结果：29 种单体酚的定量限在0.001～0.01 mg/L之间，线性相关系数R2均大于0.99，加标回收率在90.8%～104.5%之间，相对标准偏差在0.26%～7.54%之间。结论：该方法前处理简便、灵敏度高、分析时间短，精密度和准确性良好，可用于葡萄酒中29 种单体酚的同时检测。

Establishment of Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry Method for Determination of 29 Monophenols in Wine

Purpose: To establish a rapid method for simultaneous determination of 29 phenols in wine by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods: The sample was diluted with acidified methanol-water, and centrifuged at high speed. The supernatant was taken for analysis. The chromatographic separation was implemented on an ACQUITY UPLC? BEH C18 column using a mobile phase consisting of 0.1% formic acid-acetonitrile and 0.1% formic acid water. The analytes were detected using an electrospray ion source with multiple reaction monitoring in the negative ion mode. The instrumental parameters were as follows: ion source temperature (TEM) 500 ℃, electrospray voltage ?4 500 V, air curtain gas (CUR) pressure, 40 psi, collision gas medium, atomized gas pressure 60 psi, auxiliary heating pressure, 50 psi. The analysis process took 17 min. Results: The limits of quantitation (LOQs) of 29 monomeric phenols were between 0.001 and 0.01 mg/L, and the linear correlation coefficients R2 were greater than 0.99. The recoveries for spiked samples ranged between 90.8% and 104.5%, with relative standard deviations (RSDs) of 0.26% to 7.54%. Conclusion: This method is characterized by simple pretreatment, high sensitivity and fast analysis as well as good precision and accuracy, and thuscan be applied to detect 29 monophenols in wine.