Amino acids(AAs)including D-and L-enantiomers are a group of organic nitrogen species in ambient aerosol.Due to the low abundances of AAs(level of ng/m^(3))and the matrix effects by coexistent components,it is challen...Amino acids(AAs)including D-and L-enantiomers are a group of organic nitrogen species in ambient aerosol.Due to the low abundances of AAs(level of ng/m^(3))and the matrix effects by coexistent components,it is challenging to quantify AA enantiomers in ambient aerosols especially under pollution conditions.In this study,we present an optimized method for analyzing AA enantiomers in atmospheric aerosol samples including a pretreatment process and the detection by high performance liquid chromatography coupled to a fuorescence detector(HPLC-FLD).Matrix effects caused by coexistent chemicals on AA enantiomers analysis in ambient aerosol samples were investigated especially for those collected in pollution episodes.The results revealed that the determination of AA enantiomers is significantly affected by the coexistent organic carbon(as a proxy of organic matter)and water-soluble ion of NH_(4)^(+).To remove the matrix effects,we applied a pretreatment using the solid phase extraction column coupled with alkaline adjustment to sample extract.After pretreatment,18 AAs including 6 pairs of D-and L-enantiomers(i.e.,leucine,isoleucine,valine,alanine,serine,and aspartic acid)can be successfully separated and quantified in aerosol samples by HPLC-FLD.The recoveries are in the range of 67%-106%.This method was successfully applied to the urban aerosol samples from pollution and non-pollution periods for AA enantiomers determination.We suggest that the concentrations of D-AAs and the ratio of D-AA/L-AA are indicative of the contribution of bacterial sources and the infuence of biomass burning.展开更多
采用高效液相色谱法在装有大环糖肽抗生素键合相的手性柱上拆分了7种氨基带有芴甲氧羰基(fluo reny l-m ethoxycarbony l,Fm o c)保护的氨基酸对映体。比较了Fm o c-缬氨酸和相应的不带保护基的缬氨酸对映体在不同流动相体系中的色谱保...采用高效液相色谱法在装有大环糖肽抗生素键合相的手性柱上拆分了7种氨基带有芴甲氧羰基(fluo reny l-m ethoxycarbony l,Fm o c)保护的氨基酸对映体。比较了Fm o c-缬氨酸和相应的不带保护基的缬氨酸对映体在不同流动相体系中的色谱保留行为;考察了甲醇-醋酸-三乙胺流动相体系中醋酸和三乙胺的浓度以及它们二者的浓度之比对N-Fm o c氨基酸对映体拆分效果的影响。实验结果表明分离温度及流动相流速的变化也会对分离结果产生影响。该法简便快速,已成功地用于这类氨基酸的光学纯度测定。展开更多
将C_(18)柱与手性冠醚柱串联,建立了一种反相高效液相色谱法用于3种芳香族氨基酸对映体同时拆分的方法。考察了反相色谱流动相的组成、p H值、柱温、流速对对映体拆分的影响。实验结果表明,当流动相为HCl O_4-乙腈溶液(86∶14,V/V,p H 2...将C_(18)柱与手性冠醚柱串联,建立了一种反相高效液相色谱法用于3种芳香族氨基酸对映体同时拆分的方法。考察了反相色谱流动相的组成、p H值、柱温、流速对对映体拆分的影响。实验结果表明,当流动相为HCl O_4-乙腈溶液(86∶14,V/V,p H 2.0)、柱温20℃、流速0.4 m L/min时,3种氨基酸对映体可获得基线分离。进一步对比了C_(18)柱、冠醚手性柱和串联顺序不同的4种分离模式,结果表明,C_(18)柱不能拆分氨基酸对映体,仅能分离不同种类氨基酸;冠醚手性柱可分离氨基酸映体,但不同种类氨基酸色谱峰出现重叠;串联模式能实现3种氨基酸对映体的基线分离,实现双柱优势互补,而串联顺序对分离影响不大,仅影响色谱峰的峰形。展开更多
基金supported by the Natural Science Foundation of China (No.41975156)。
文摘Amino acids(AAs)including D-and L-enantiomers are a group of organic nitrogen species in ambient aerosol.Due to the low abundances of AAs(level of ng/m^(3))and the matrix effects by coexistent components,it is challenging to quantify AA enantiomers in ambient aerosols especially under pollution conditions.In this study,we present an optimized method for analyzing AA enantiomers in atmospheric aerosol samples including a pretreatment process and the detection by high performance liquid chromatography coupled to a fuorescence detector(HPLC-FLD).Matrix effects caused by coexistent chemicals on AA enantiomers analysis in ambient aerosol samples were investigated especially for those collected in pollution episodes.The results revealed that the determination of AA enantiomers is significantly affected by the coexistent organic carbon(as a proxy of organic matter)and water-soluble ion of NH_(4)^(+).To remove the matrix effects,we applied a pretreatment using the solid phase extraction column coupled with alkaline adjustment to sample extract.After pretreatment,18 AAs including 6 pairs of D-and L-enantiomers(i.e.,leucine,isoleucine,valine,alanine,serine,and aspartic acid)can be successfully separated and quantified in aerosol samples by HPLC-FLD.The recoveries are in the range of 67%-106%.This method was successfully applied to the urban aerosol samples from pollution and non-pollution periods for AA enantiomers determination.We suggest that the concentrations of D-AAs and the ratio of D-AA/L-AA are indicative of the contribution of bacterial sources and the infuence of biomass burning.
文摘采用高效液相色谱法在装有大环糖肽抗生素键合相的手性柱上拆分了7种氨基带有芴甲氧羰基(fluo reny l-m ethoxycarbony l,Fm o c)保护的氨基酸对映体。比较了Fm o c-缬氨酸和相应的不带保护基的缬氨酸对映体在不同流动相体系中的色谱保留行为;考察了甲醇-醋酸-三乙胺流动相体系中醋酸和三乙胺的浓度以及它们二者的浓度之比对N-Fm o c氨基酸对映体拆分效果的影响。实验结果表明分离温度及流动相流速的变化也会对分离结果产生影响。该法简便快速,已成功地用于这类氨基酸的光学纯度测定。
文摘将C_(18)柱与手性冠醚柱串联,建立了一种反相高效液相色谱法用于3种芳香族氨基酸对映体同时拆分的方法。考察了反相色谱流动相的组成、p H值、柱温、流速对对映体拆分的影响。实验结果表明,当流动相为HCl O_4-乙腈溶液(86∶14,V/V,p H 2.0)、柱温20℃、流速0.4 m L/min时,3种氨基酸对映体可获得基线分离。进一步对比了C_(18)柱、冠醚手性柱和串联顺序不同的4种分离模式,结果表明,C_(18)柱不能拆分氨基酸对映体,仅能分离不同种类氨基酸;冠醚手性柱可分离氨基酸映体,但不同种类氨基酸色谱峰出现重叠;串联模式能实现3种氨基酸对映体的基线分离,实现双柱优势互补,而串联顺序对分离影响不大,仅影响色谱峰的峰形。
