A β-cyclodextrin derivative, perbenzyl-β-cyclodextrin, was prepared and used as a chiral stationary phase for capillary gas chromatography. Using FID detector and the column temperature between 70 and 80℃, the chir...A β-cyclodextrin derivative, perbenzyl-β-cyclodextrin, was prepared and used as a chiral stationary phase for capillary gas chromatography. Using FID detector and the column temperature between 70 and 80℃, the chiral separations of racemic 3-phenyl-1, 2-epoxyethane and 1-phenyl-1-propanol on a 14m×0.23mm I. D. fused silica column with the β-cyclodextrin derivative were carried out and the optical purities of optically active 1-phenyl-1-propanol samples prepared by asymmetric synthesis were determined.展开更多
建立了一种μ-QuEChERS结合气相色谱-三重四极杆串联质谱仪(gas chromatography-triple quadrupole tandem mass spectrometry,GC-MS/MS)在10 min内测定桃胶中106种农药残留的方法。样品经μ-QuEChERS方法提取、净化,经超高惰性气相色谱...建立了一种μ-QuEChERS结合气相色谱-三重四极杆串联质谱仪(gas chromatography-triple quadrupole tandem mass spectrometry,GC-MS/MS)在10 min内测定桃胶中106种农药残留的方法。样品经μ-QuEChERS方法提取、净化,经超高惰性气相色谱柱(highly inert gas chromatographic column,HIGC)分离,以三重四极杆-串联质谱仪检测分析,基质标准曲线外标法定量。106种农药在0.00200~0.400 mg/kg范围,其线性相关系数R均大于0.995,对于0.500 g样品的106种农药的检出限为(5.84×10^(-6))~(2.81×10^(-3))mg/kg,定量限为(1.95×10^(-5))~(9.36×10^(-3))mg/kg,且低、中、高3个浓度添加水平的回收率为72%~109%,相对标准偏差(relative standard deviations,RSDs)为0.73%~10%。该方法具有快捷、污染小、可靠性强的特点,适用于桃胶中多种农药残留的快速定性和定量检测。展开更多
Troxerutin(TRO)is a mixture of semi-synthetic flavonoids prepared by hydroxyethylation of rutin,and it is commonly used for the treatment of cerebrovascular diseases.The main active ingredient is trishydroxyethyl ruti...Troxerutin(TRO)is a mixture of semi-synthetic flavonoids prepared by hydroxyethylation of rutin,and it is commonly used for the treatment of cerebrovascular diseases.The main active ingredient is trishydroxyethyl rutin.The mother liquor of TRO contains a lot of TRO and other derivatives of hydroxyethylated rutin.In order to make full use of the mother liquor of TRO,an efficient method was developed for recovering high-purity TRO from mother liquor of TRO by combining silica gel column chromatography with semi-preparative liquid chromatography.In the silica gel column chromatographic separation,the ratio of silica gel to sample and eluent composition were investigated to obtain optimum separation effect.The results showed that when the ratio of silica gel to sample was 50,and acetone–ethyl acetate–water–glacial acetic acid(10:10:3:1,v/v/v/v)was used as the eluent,the separation effect of TRO and adjacent impurities was good.Moreover,150 g of TRO with a purity of 80%could be obtained from 1 kg of mother liquor of TRO by the silica gel column chromatographic separation,and the results were consistent with the quality standard of TRO raw material.Subsequently,the semi-preparative HPLC was performed,and 100 g TRO with a purity of up to 98%(w/w)was obtained.Meanwhile,tetrahydroxyethylrutin and tetrahydroxyethylquercetin with purity greater than 98%were obtained.This work proposed the separation and preparation of TRO with high-purity from the production waste of TRO for the first time,which had certain environmental benefits and economic benefits.展开更多
文摘A β-cyclodextrin derivative, perbenzyl-β-cyclodextrin, was prepared and used as a chiral stationary phase for capillary gas chromatography. Using FID detector and the column temperature between 70 and 80℃, the chiral separations of racemic 3-phenyl-1, 2-epoxyethane and 1-phenyl-1-propanol on a 14m×0.23mm I. D. fused silica column with the β-cyclodextrin derivative were carried out and the optical purities of optically active 1-phenyl-1-propanol samples prepared by asymmetric synthesis were determined.
文摘建立了一种μ-QuEChERS结合气相色谱-三重四极杆串联质谱仪(gas chromatography-triple quadrupole tandem mass spectrometry,GC-MS/MS)在10 min内测定桃胶中106种农药残留的方法。样品经μ-QuEChERS方法提取、净化,经超高惰性气相色谱柱(highly inert gas chromatographic column,HIGC)分离,以三重四极杆-串联质谱仪检测分析,基质标准曲线外标法定量。106种农药在0.00200~0.400 mg/kg范围,其线性相关系数R均大于0.995,对于0.500 g样品的106种农药的检出限为(5.84×10^(-6))~(2.81×10^(-3))mg/kg,定量限为(1.95×10^(-5))~(9.36×10^(-3))mg/kg,且低、中、高3个浓度添加水平的回收率为72%~109%,相对标准偏差(relative standard deviations,RSDs)为0.73%~10%。该方法具有快捷、污染小、可靠性强的特点,适用于桃胶中多种农药残留的快速定性和定量检测。
基金Shaanxi science and technology hall project(Grant No.2018JM7060)Provincial Key Discipline Construction Project of pharmacy of Xi’an Medical University(Grant No.2016YXXK08)。
文摘Troxerutin(TRO)is a mixture of semi-synthetic flavonoids prepared by hydroxyethylation of rutin,and it is commonly used for the treatment of cerebrovascular diseases.The main active ingredient is trishydroxyethyl rutin.The mother liquor of TRO contains a lot of TRO and other derivatives of hydroxyethylated rutin.In order to make full use of the mother liquor of TRO,an efficient method was developed for recovering high-purity TRO from mother liquor of TRO by combining silica gel column chromatography with semi-preparative liquid chromatography.In the silica gel column chromatographic separation,the ratio of silica gel to sample and eluent composition were investigated to obtain optimum separation effect.The results showed that when the ratio of silica gel to sample was 50,and acetone–ethyl acetate–water–glacial acetic acid(10:10:3:1,v/v/v/v)was used as the eluent,the separation effect of TRO and adjacent impurities was good.Moreover,150 g of TRO with a purity of 80%could be obtained from 1 kg of mother liquor of TRO by the silica gel column chromatographic separation,and the results were consistent with the quality standard of TRO raw material.Subsequently,the semi-preparative HPLC was performed,and 100 g TRO with a purity of up to 98%(w/w)was obtained.Meanwhile,tetrahydroxyethylrutin and tetrahydroxyethylquercetin with purity greater than 98%were obtained.This work proposed the separation and preparation of TRO with high-purity from the production waste of TRO for the first time,which had certain environmental benefits and economic benefits.
