超高效合相色谱对植物油中角鲨烯的快速测定及方法比较

建立超高效合相色谱(ultra performance convergence chromatography,UPC~2)分离和测定植物油中角鲨烯的方法。样品经正己烷溶解过滤后直接进样分析;流动相以CO2为主体,乙腈为助溶剂;色谱柱Acquity UPC~2 HSS C_(18) SB(3.0 mm×100 mm,1.7 μm),流速1.5 mL/min,检测波长215 nm,动态背压12.4 MPa,柱温50℃,进样量1.0 μL。角鲨烯在2.5 min内实现完全分离,并在0.53～105.00 mg/L的范围内具有良好的线性(r0.999 1);回收率为86.97%～102.41%;相对标准偏差为1.3%～4.1%(n=8);方法检出限(RSN=3)为0.53 mg/L。通过UPC2与超高效液相色谱对实际样品的分析及不同前处理方法的比较,结果表明,UPC_2方法具高效快速、操作简单、实验成本低等优点,可以满足植物油中角鲨烯的快速、高通量检测。

Rapid Determination of Squalene in Vegetable Oils by Ultra Performance Convergence Chromatography and Comparison with Ultra-Performance Liquid Chromatography

An ultra-performance convergence chromatography (UPC2) method was developed and validated for the determination of squalene in vegetable oils. The sample was dissolved in n-hexane, and analyzed directly after filtration. Optimum separation was achieved on a UPC2 HSS C18 SB column (3.0 mm × 100 mm, 1.7 μm) with gradient elution at a flow rate of 1.5 mL/min. Other parameters were set as follows: back pressure 12.4 MPa, column temperature 50 ℃, injection volume 1.0 μL, and detection wavelength 215 nm. The results showed that complete separation of the analyte was accomplished within 2.5 min, and the method had a good linearity in the range of 0.53-105.00 mg/L (r > 0.999 1). The recovery was between 86.97% and 102.41% with relative standard deviation ranging from 1.3% to 4.1% (n = 8). The limit of detection (RSN = 3) was 0.53 mg/L for squalene. The use of UPC2 with different sample pre-treatment methods to detect actual samples was compared with ultra-performance liquid chromatography (UPLC). The results showed that UPC2 was more efficient, faster, simpler and cheaper, which could be useful for the rapid and high throughput detection of squalene in oil.