分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2014年
5期
723-728
,共6页
欧阳新平%陈子龙%邱学青
歐暘新平%陳子龍%邱學青
구양신평%진자룡%구학청
木质素%氧化降解%单酚类化合物%超高效液相色谱%高分辨质谱
木質素%氧化降解%單酚類化閤物%超高效液相色譜%高分辨質譜
목질소%양화강해%단분류화합물%초고효액상색보%고분변질보
Lignin%Oxidative degradation%Monomeric phenols%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。
建立瞭木質素氧化降解產物中單酚類產物的超高效液相色譜/高分辨質譜聯用( UPLC/HRMS)檢測方法。採用反相C18色譜柱,柱溫30℃,0.1%(V/V)甲痠溶液-10%(V/V)甲醇乙腈溶液為流動相二元梯度洗脫,流速為0.2 mL/min,280 nm波長下紫外檢測,可實現木質素氧化降解穫得的9種單酚類化閤物的有效分離,結閤電噴霧離子源超高分辨飛行時間質譜( ESI-Q-TOF)正離子模式進行檢測,對單酚類降解產物進行準確定性分析;通過高分辨質譜精確離子流抽提,麵積外標法定量分析。本方法的線性範圍為5.0~10000μg/L,線性相關繫數大于0.9998,相對標準偏差(RSD)小于1.7%,檢齣限(LOD)和定量限(LOQ)分彆為0.1~0.3μg/L和0.3~0.5μg/L,平均加標迴收率為98.9%~105.1%。結果錶明,痠性流動相體繫下的正離子模式進行單酚類產物的質譜分析,具有較好的色譜分離效果和較高靈敏度。
건립료목질소양화강해산물중단분류산물적초고효액상색보/고분변질보련용( UPLC/HRMS)검측방법。채용반상C18색보주,주온30℃,0.1%(V/V)갑산용액-10%(V/V)갑순을정용액위류동상이원제도세탈,류속위0.2 mL/min,280 nm파장하자외검측,가실현목질소양화강해획득적9충단분류화합물적유효분리,결합전분무리자원초고분변비행시간질보( ESI-Q-TOF)정리자모식진행검측,대단분류강해산물진행준학정성분석;통과고분변질보정학리자류추제,면적외표법정량분석。본방법적선성범위위5.0~10000μg/L,선성상관계수대우0.9998,상대표준편차(RSD)소우1.7%,검출한(LOD)화정량한(LOQ)분별위0.1~0.3μg/L화0.3~0.5μg/L,평균가표회수솔위98.9%~105.1%。결과표명,산성류동상체계하적정리자모식진행단분류산물적질보분석,구유교호적색보분리효과화교고령민도。
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.