超高效液相色谱/高分辨质谱法测定木质素氧化降解产物中单酚类化合物

Determination of Monophenolic Compounds from Lignin Oxidative Degradation Using Ultra Performance Liquid Chromatography /High Resolution Mass Spectrometry

建立了木质素氧化降解产物中单酚类产物的超高效液相色谱/高分辨质谱联用（ UPLC/HRMS）检测方法。采用反相C18色谱柱,柱温30℃,0.1%（V/V）甲酸溶液-10%（V/V）甲醇乙腈溶液为流动相二元梯度洗脱,流速为0.2 mL/min,280 nm波长下紫外检测,可实现木质素氧化降解获得的9种单酚类化合物的有效分离,结合电喷雾离子源超高分辨飞行时间质谱（ ESI-Q-TOF）正离子模式进行检测,对单酚类降解产物进行准确定性分析；通过高分辨质谱精确离子流抽提,面积外标法定量分析。本方法的线性范围为5.0~10000μg/L,线性相关系数大于0.9998,相对标准偏差（RSD）小于1.7%,检出限（LOD）和定量限（LOQ）分别为0.1~0.3μg/L和0.3~0.5μg/L,平均加标回收率为98.9%~105.1%。结果表明,酸性流动相体系下的正离子模式进行单酚类产物的质谱分析,具有较好的色谱分离效果和较高灵敏度。

A method for the determination of monophenolic compounds derived from oxidative degradation of lignin was developed by combination of ultra performance liquid chromatography with high resolution mass spectrometry （ UPLC-HRMS） . The efficient separation of nine monophenolic compounds was carried out on a RP C18 column with the mobile phase of 0. 1% （V/V） formic acid aquous-10% （V/V） methnol/acetonitrile at 30 ℃ at a flow rate of 0. 2 mL/min, and the detection wavelength was 280 nm. Electrospray ionization coupled with high resolution time of flight mass spectrometry （ ESI-Q-TOF） under positive ionization mode was used for the qualitative identification of monophenolic compounds degraded from lignin. The quantitative analysis was performed with external standard method based on high resolution extracted ion chromatography. The linear ranges were 5 . 0-10000 μg/L with correlation of more than 0 . 9998 . The LODs and LOQs were 0. 1-0. 3 μg/L and 0. 3-0. 5 μg/L, respectively. The average recoveries were 98. 9. 1%-105. 11% with less than relative standard deviations of 1. 7%. The method is rapid,sensitive and easy to operate.