超高效合相色谱串联四级杆飞行时间质谱定性分析中/长链结构甘油三酯组成

Characteristics of Triacylglycerols Composition of Medium/Long Chain Structured Triacylglycerols by Ultraperformance Convergence Chromatography Combined with A Quadrupole Time-of-flight Mass Spectrometry

目的建立一种超高效合相色谱串联四级杆飞行时间质谱定性分析(UPCC-QTOF-MS)中/长链结构甘油三酯组成的方法。方法采用Acquity UPCC HSS C18SB色谱柱(3.0 mm×150 mm,1.8μm),以CO_2和甲醇-乙腈(7∶3,V/V)为流动相,梯度洗脱,柱温28℃,流速1.2 mL·min^(-1),背压117.2 MPa,以含0.1%甲酸和2 mmol·L^(-1)甲酸铵的甲醇为补充溶剂;电喷雾电离正离子连同MSE技术一、二级精确扫描,精确采集分子离子和碎片离子信息,对各甘油三酯组分进行准确结构确证。结果得到分离良好的52种甘油三酯组分,并分别进行了准确结构确证。结论该法分离能力强、定性结果准确且绿色环保,是中/长链结构甘油三酯质量控制的有效分析方法。

OBJECTIVE To develop a method suitable for rapid and accurate analysis of triacylglycerols in medium/long chain structured triacylglycerols by uhraperformance convergence chromatography combined with a quadrupole time-of-flight mass spectrometry. METHODS The separation was performed at 28 ℃ on a Waters Acquity UPCC system by anHSS C18 SB column （3.0 mm× 150 mm,1.8 μm） with gradient elutionof CO2 and methanol acetonitrile （7： 3, V/V） ,the flow rate was 1.2 mL min-1, the back pressure was 117.2 MPa, and methanol containing 0. 1% formic acid and 2 mmol L-1 ammonium formate was used as supplement solvent. Positive ion electrospray ionisation （ESI） mode and MSE technology were used in which two sep- arate scan functions were programmed for the MS acquisition. The qualitative analyses were carried out by using precise mass in- formation of parent ions and product ions. RESULTS A total of 52 triacylglycerols were obtained and their stuctures were iden- tified by analyzing the precise mass information of their parent ions and product ions respectively. CONCLUSION The method is simple, highly accurate, and environmental friendly with good resolution, and can be used for rapid and accurate analysis of medium/long chain triacylglycerols excipients.