目的: 建立超临界流体色谱方法同时测定甲酚皂溶液中3个甲酚异构体的含量。方法: 采用ACQUITY UPC2 TrefoilTM CEL1(150 mm×3.0 mm,2.5 μm)色谱柱,流动相为二氧化碳-甲醇,梯度洗脱,流速2 mL·min-1,柱温30 ℃,样品室温15 ℃,背压11.7 MPa,检测波长278 nm,进样量1 μL。结果: 甲酚皂溶液中邻甲酚、间甲酚和对甲酚在3 min内实现分离,相邻主峰间的分离度分别为5.8和7.4。邻甲酚、间甲酚和对甲酚的检测限均为0.8 μg·mL-1,定量限均为2.0 μg·mL-1,线性范围均为4~200 μg·mL-1(r=0.999 9,n=6),平均加标回收率分别为99.0%(n=9),97.5%(n=9)和98.4%(n=9),3批甲酚皂溶液中含甲酚分别为86.8%、86.9%和87.2%。结论: 建立的超临界流体色谱方法能快速分离甲酚的3个异构体,操作简单,且极大幅度减少有机溶剂使用量,绿色环保,准确度高,重现性好,可用于甲酚皂溶液中甲酚的含量测定。
Objective: To establish a supercritical fluid chromatography method for the separation of cresol isomers in saponated cresol solution, meanwhile assaying the three isomers. Methods: Three cresol isomers of saponated cresol solution were separated on a ACQUITY UPC2 TrefoilTM CEL1 column (150 mm×3.0 mm, 2.5 μm) main tained at 30 ℃ with the mobile phase containing a mixture of CO2 and methanol at 2 mL·min-1,and the detection wavelength was set at 278 nm. The sample was kept at 15 ℃.The back pressure was set at 11.7 MPa. The injection volume was 1 μL. Results: The o-cresol, m-cresol and p-cresol were separated successfully in 3 min using the proposed method, and the resolutions between the closely peaks were 5.8 and 7.4 respectively. The limit of detection (S/N=3) was 0.8 μg·mL-1 and the limit of quantitative (S/N=10) was 2.0 μg·mL-1. Good linear relationship was established between the peak response and the concentration in the range of 4-200 μg·mL-1 for all isomers (r2=0.999 9, n=6). The spiked recoveries of three isomers (o-cresol, m-cresol and p-cresol) was found to be acceptable for 99.0%, 97.5%, 98.4%, respectively. The contents of cresol in three saponated cresol solution were 86.8%, 86.9% and 87.2%, respectively. Conclusion: The proposed method resolves the difficulty in separating cresol isomers and reduce sharply volumes of organic solvents, showing fast, high accuracy, repeatability and environmentally friendly. It can be employed for the assay of the cresol in saponated cresol solution.
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