CAJ | 학술논문

采用超高效合相色谱_质谱( UPC2_MS)技术,建立了工业油酸中5种常见的脂肪酸(软脂酸、硬脂酸、油酸、亚油酸和亚麻酸)的快速检测方法。样品用正己烷溶解,采用超临界CO2_甲醇/乙腈(1∶1, V/V)梯度洗脱,经Acquity UPC2 BEH 2_EP色谱柱(100 mm ×2.1 mm,1.7μm)分离,通过质谱检测器在负离子电喷雾模式下对目标化合物进行分析,外标法定量。通过对UPC2_MS条件的优化,5种脂肪酸在3 min内实现有效分离,目标物在0.5~100 mg/L 范围内具有良好的线性(相关系数大于0.9985)；在3个添加水平下,5种脂肪酸的回收率在89.3%~106.7%之间,相对标准偏差为0.8%~3.0%；方法检出限(S/N≥3)为0.07~0.26 mg/L。实际样品分析结果表明,本方法不但简单快速,分离效果好,而且无需对脂肪酸样品进行衍生化,同时为UPC2在油脂类相关领域的研究与开发提供一种快速有效的检测方法。
채용초고효합상색보_질보( UPC2_MS)기술,건립료공업유산중5충상견적지방산(연지산、경지산、유산、아유산화아마산)적쾌속검측방법。양품용정기완용해,채용초림계CO2_갑순/을정(1∶1, V/V)제도세탈,경Acquity UPC2 BEH 2_EP색보주(100 mm ×2.1 mm,1.7μm)분리,통과질보검측기재부리자전분무모식하대목표화합물진행분석,외표법정량。통과대UPC2_MS조건적우화,5충지방산재3 min내실현유효분리,목표물재0.5~100 mg/L 범위내구유량호적선성(상관계수대우0.9985)；재3개첨가수평하,5충지방산적회수솔재89.3%~106.7%지간,상대표준편차위0.8%~3.0%；방법검출한(S/N≥3)위0.07~0.26 mg/L。실제양품분석결과표명,본방법불단간단쾌속,분리효과호,이차무수대지방산양품진행연생화,동시위UPC2재유지류상관영역적연구여개발제공일충쾌속유효적검측방법。
A rapid method was developed for the determination of 5 common fatty acids, palmitic acid, stearic acid, oleic acid, linoleic acid and linolenic acid in industrial oleic acid based on ultra_performance convergence chromatography_mass spectrometry ( UPC_MS) . The sample was dissolved by n_hexane, followed by clean_up of extract using 0. 22 μm organic phase filter. The fatty acids were separated in 3 min on the column of Acquity UPC2 BEH 2_EP by gradient elution with carbon dioxide and methanol/acetonitrile (1∶1, V/V) system, and finally detected by MS detector in ESI- mode. Through the optimization of UPC2_MS condition, the reasonable linearity was achieved for all the analytes over the range of 0. 5-100 mg/L with the correlation coefficients ( R2 ) greater than 0. 9985. The recoveries for five fatty acids at three spiked levels were in the range from 89 . 3% to 106 . 67% with relative standard deviations of 0 . 8%-3 . 0%. The limits of detection for target compounds in the method ranged from 0. 07 mg/L to 0. 26 mg/L. The real sample analysis showed that this method was simple,fast and had a good separation effect. There was no need of derivatization for fatty acid samples. This work would provide a fast and effective detection method for UPC2 technology in oil related research field.