Separation and Determination of Positional Isomers 1-Naphthol and 2-Naphthol by Chiral Stationary Phase Gas Chromatography
Separation of the positional isomers 1-naphthol and 2-naphthol by gas chromatography is a difficult task,especially for the determination of trace amounts of 2-naphthol impurities in 1-naphthol,which can be easily interfered with.Therefore,it is particularly necessary to establish an accurate and robust separation and determination method for the purity control of 1-naphthol and 2-naphthol.Based on the special selectivity of chiral stationary phases,a gas chromatographic method for the separation of positional isomers 1-naphthol and 2-naphthol was developed,and the effects of carrier gas linear velocity,column temperature,temperature increase rate,split ratio and injection volume on the separation of 1-naphthol and 2-naphthol were also investigated,and the method was applied to the determination of real samples.A cyclodextrin-based chiral column,SH-bDEXsa,was used for the analysis and a hydrogen flame ionisation detector for the detection.Under the optimized optimal chromatographic conditions:carrier gas linear velocity of 60 cm/s,initial column temperature of 180℃,ramp rate of 7℃/min,injection volume of 1 μL,and separation ratio of 9,the separation of 1-naphthol and 2-naphthol could be achieved in less than 7 min,and the separation was much more than 1.5.1-naphthol and 2-naphthol exhibited good linearity over the concentration range of 1.0 μg/mL～100.0 μg/mL,and the correlation coefficients were both greater than 0.999.The correlation coefficients were greater than 0.999.The limits of detection(LOD)were 0.27 μg/mL and the limits of quantification(LOQ)were 0.91 and 0.90 μg/mL for 1-naphthol and 2-naphthol,respectively.The recoveries of 1-naphthol and 2-naphthol at three different spiked concentration levels,1.0,5.0,and 20.0 μg/mL,with methanol as the blank substrate ranged from 93.1%to 104.6%and 90.4%to 113.3%,respectively.90.4%～113.2%with the relative standard deviations(RSDs)of 0.58%～4.70%and 1.19%～2.67%,respectively.The method is simple,fast and can be used for the determination of the purity of 1-naphthol or 2-naphthol and the determination of the impurity content of isomers.
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