摘要
气相色谱法分离位置异构体1-萘酚和2-萘酚是一个难点,尤其是测定1-萘酚中微量的2-萘酚杂质时,2-萘酚容易受到干扰。因此,建立一种准确、鲁棒性好的分离及测定方法,对1-萘酚和2-萘酚的纯度控制显得尤为必要。基于手性固定相的特殊选择性,建立了分离位置异构体1-萘酚和2-萘酚的气相色谱方法,同时考察了载气线速度、柱温、升温速率、分流比及进样量对1-萘酚和2-萘酚分离度的影响,并将该方法应用于实际样品的测定。采用环糊精类手性色谱柱SH-bDEXsa进行分析,氢火焰离子化检测器进行检测。在优化后的最佳色谱条件下:载气线速度60 cm/s,初始柱温180℃,升温速率7℃/min,进样量1μL,分离比9,1-萘酚和2-萘酚可在7 min之内实现分离,且分离度远大于1.5。1-萘酚和2-萘酚在1.0μg/mL~100.0μg/mL的浓度范围内,线性关系良好,相关系数均大于0.999,1-萘酚和2-萘酚的检出限均为0.27μg/mL,定量限分别为0.91和0.90μg/mL。以甲醇作为空白基质,1-萘酚和2-萘酚在1.0、5.0、20.0μg/mL 3个不同加标浓度水平下的回收率分别为93.1%~104.6%和90.4%~113.2%,相对标准偏差(RSD)分别为0.58%~4.70%和1.19%~2.67%。本方法简单、速度快,可用于1-萘酚或2-萘酚纯度测定及异构体杂质含量测定。
Separation of the positional isomers 1-naphthol and 2-naphthol by gas chromatography is a difficult task,especially for the determination of traceamounts of 2-naphthol impurities in 1-naphthol,which can be easily interfered with.Therefore,it is particularly necessary to establish an accurate and robustseparation and determination method for the purity control of 1-naphthol and 2-naphthol.Based on the special selectivity of chiral stationary phases,a gaschromatographic method for the separation of positional isomers 1-naphthol and 2-naphthol was developed,and the effects of carrier gas linear velocity,columntemperature,temperature increase rate,split ratio and injection volume on the separation of 1-naphthol and 2-naphthol were also investigated,and the method wasapplied to the determination of real samples.A cyclodextrin-based chiral column,SH-bDEXsa,was used for the analysis and a hydrogen flame ionisation detector forthe detection.Under the optimized optimal chromatographic conditions:carrier gas linear velocity of 60 cm/s,initial column temperature of 180℃,ramp rate of7℃/min,injection volume of 1μL,and separation ratio of 9,the separation of 1-naphthol and 2-naphthol could be achieved in less than 7 min,and the separationwas much more than 1.5.1-naphthol and 2-naphthol exhibited good linearity over the concentration range of 1.0μg/mL~100.0μg/mL,and the correlationcoefficients were both greater than 0.999.The correlation coefficients were greater than 0.999.The limits of detection(LOD)were 0.27μg/mL and the limits ofquantification(LOQ)were 0.91 and 0.90μg/mL for 1-naphthol and 2-naphthol,respectively.The recoveries of 1-naphthol and 2-naphthol at three different spikedconcentration levels,1.0,5.0,and 20.0μg/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 thedetermination of the purity of 1-naphthol or^(2)-naphthol and the determination of the impurity content of isomers.
作者
张振永
Zhang Zhenyong(Shimadzu(Shanghai)Global Laboratory Consumables Co.,Ltd.,Shanghai 200233,China)
出处
《广东化工》
CAS
2024年第23期129-132,共4页
Guangdong Chemical Industry
关键词
手性固定相
气相色谱法
位置异构体
1-萘酚
2-萘酚
chiral stationary phase
gas chromatography
positional isomers
1-naphthol
2-naphthol
作者简介
张振永(1992-),男,河南濮阳人,硕士,主要研究方向为色谱质谱分析。
