泡沫浮选和固相萃取在分离富集人参皂苷和激素中的应用
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摘要
本文研究了泡沫浮选和固相萃取在分离富集人参皂苷和激素方面的应用。
将泡沫浮选与固相萃取联用，分离富集三七萃取溶液中的三七和人参皂苷，实现了二醇组皂苷和三醇组皂苷的分离。
发现了离子液体的起泡特性，将其运用到泡沫浮选-固相萃取中，研究了影响离子液体起泡能力的各种因素和规律。并用该方法分离富集了雨水和湖水中的十四种激素，萃取方法简便快速，结果令人满意。
将离子液体泡沫浮选与液液微萃取相结合，分离富集了水样中的一些激素。考察了离子液体泡沫浮选和离子液体液液微萃取的影响因素，灵敏度和选择性均较好。
用基质固相分散萃取高效液相质谱法分离富集测定了饲料和鹿茸中的激素，考察了分析条件对分析性能的影响，建立了分析方法。
The application of foam floatation and solid phase extraction in separation andconcentration of ginsenosides and hormones was investigated in this thesis.
A foam floatation (FF) and a solid phase extraction(SPE) were synchronouslyapplied to the separation and concentration of notoginsenoside R1and ginsenosidesRg1、Re、Rb1、Rc、Rb2、Rb3and Rd from extract of Panax notoginsen (Burk.) F.H.Chen. The analytes are separated and determined by liquid chromatography. Theselectivity and sensitivity for the determination of the ananlytes were improved. Theexperimental conditions, including the flow rate of nitrogen gas, floatation time andpH value of sample solution for FF and elution conditions for SPE were examined andoptimized. Average recoveries for protopanaxdiol (PPD) ginsenosides Rb1, Rc, Rb2,Rb3and Rd are between84.5%and98.8%and for notoginsenoside R1is85.01%.But average recoveries for protopanaxtriol (PPT) ginsenosides Rg1and Re are verylow. The relative standard deviations (RSDs) are lower than6.73%for the PPDginsenosides. The experimental results indicated that the proposed method is sampleand effective for the separation and concentration of the low content ofnotoginsenoside and ginsenosides in extracts from Panax notoginsen (Burk.) F.H.Chen., but also of great potential for the separation of PPD and PPT.
The foaming property of ionic liquids (ILs) was found and the factors that caninfluence foamability of the ILs were investigated. Based on the foaming property ofthe ILs, the foam floatation-solid phase extraction (FF-SPE) is developed. TheIL-based FF-SPE is applied to the extraction and concentration of14steroid hormones in water samples and the steroid hormones are determined byhigh-performance liquid chromatography. Some experimental conditions areexamined and optimized. The extraction and concentration are performedsynchronously in ten minutes. The recoveries of the hormones range from50.6to95.2%for lake water sample and from53.4to98.7%for rain water sample. Theintra-day precision ranged from2.43to7.43%and from2.07to7.01%for the lakewater and rain water sample, respectively. Compared with other extraction methods,the IL-based FF-SPE is rapid, sample and low contamination.
The foaming property of ILs is also applied to the FF. The IL-based FF followedby liquid-liquid microextraction(LLME) is developed and applied to separate andconcentrate estradiol benzoate,17-α-estradiol and quinestrol in water sample. And theanalytes are separated and determined by high performance liquid chromatographyequipped with fluorescence detector. The experimental factors, the concentration offloatation solvent, flow rate of nitrogen gas and floatation time for FF and the kindand volume of extraction solvent, concentration of salt, centrifugation and vibrationtime for LLME are investigated. The Detection Limit of estradiol benzoate,17-α-estradiol and quinestrol was reduced greatly, and the sensitivity and theselectivity are both good in this work.
The Matrix solid-phase dispersion extraction was used to separated andconcentrated the hormones from feeds and antler velvet.The high-performance liquidchromatography mass spectrometry was applied to the determination of the hormones.The influence factors including dispersant type, ratio of samples to dispersant, typesand volume of elution solvent are investigated. The results indicated that theextraction efficiency of fourteen kinds of hormones were highest when the ratio ofsamples to dispersant is1:4and30mL methanol-water solution(V:V=4:1) wasselected as the elution solvent. The extraction solution was evaporated to dryness,dissolved by1.0mL of methanol, filtered through0.45μm filter and then analyzed byliquid chromatography-electrospray ionization mass spectrometry. The establishedmethod can achieve the extraction and purification of the target analyte in one step.The result indicates there are many virtues for this method, such as high purificationefficiency, less analytical time, and small amount of sample and solvent. In addition,the recoveries of the analytes range from83.40to99.17%and RSDs are lower than7.42%. The LODs are lower than7.00ng kg-1.
将泡沫浮选与固相萃取联用，分离富集三七萃取溶液中的三七和人参皂苷，实现了二醇组皂苷和三醇组皂苷的分离。
发现了离子液体的起泡特性，将其运用到泡沫浮选-固相萃取中，研究了影响离子液体起泡能力的各种因素和规律。并用该方法分离富集了雨水和湖水中的十四种激素，萃取方法简便快速，结果令人满意。
将离子液体泡沫浮选与液液微萃取相结合，分离富集了水样中的一些激素。考察了离子液体泡沫浮选和离子液体液液微萃取的影响因素，灵敏度和选择性均较好。
用基质固相分散萃取高效液相质谱法分离富集测定了饲料和鹿茸中的激素，考察了分析条件对分析性能的影响，建立了分析方法。
The application of foam floatation and solid phase extraction in separation andconcentration of ginsenosides and hormones was investigated in this thesis.
A foam floatation (FF) and a solid phase extraction(SPE) were synchronouslyapplied to the separation and concentration of notoginsenoside R1and ginsenosidesRg1、Re、Rb1、Rc、Rb2、Rb3and Rd from extract of Panax notoginsen (Burk.) F.H.Chen. The analytes are separated and determined by liquid chromatography. Theselectivity and sensitivity for the determination of the ananlytes were improved. Theexperimental conditions, including the flow rate of nitrogen gas, floatation time andpH value of sample solution for FF and elution conditions for SPE were examined andoptimized. Average recoveries for protopanaxdiol (PPD) ginsenosides Rb1, Rc, Rb2,Rb3and Rd are between84.5%and98.8%and for notoginsenoside R1is85.01%.But average recoveries for protopanaxtriol (PPT) ginsenosides Rg1and Re are verylow. The relative standard deviations (RSDs) are lower than6.73%for the PPDginsenosides. The experimental results indicated that the proposed method is sampleand effective for the separation and concentration of the low content ofnotoginsenoside and ginsenosides in extracts from Panax notoginsen (Burk.) F.H.Chen., but also of great potential for the separation of PPD and PPT.
The foaming property of ionic liquids (ILs) was found and the factors that caninfluence foamability of the ILs were investigated. Based on the foaming property ofthe ILs, the foam floatation-solid phase extraction (FF-SPE) is developed. TheIL-based FF-SPE is applied to the extraction and concentration of14steroid hormones in water samples and the steroid hormones are determined byhigh-performance liquid chromatography. Some experimental conditions areexamined and optimized. The extraction and concentration are performedsynchronously in ten minutes. The recoveries of the hormones range from50.6to95.2%for lake water sample and from53.4to98.7%for rain water sample. Theintra-day precision ranged from2.43to7.43%and from2.07to7.01%for the lakewater and rain water sample, respectively. Compared with other extraction methods,the IL-based FF-SPE is rapid, sample and low contamination.
The foaming property of ILs is also applied to the FF. The IL-based FF followedby liquid-liquid microextraction(LLME) is developed and applied to separate andconcentrate estradiol benzoate,17-α-estradiol and quinestrol in water sample. And theanalytes are separated and determined by high performance liquid chromatographyequipped with fluorescence detector. The experimental factors, the concentration offloatation solvent, flow rate of nitrogen gas and floatation time for FF and the kindand volume of extraction solvent, concentration of salt, centrifugation and vibrationtime for LLME are investigated. The Detection Limit of estradiol benzoate,17-α-estradiol and quinestrol was reduced greatly, and the sensitivity and theselectivity are both good in this work.
The Matrix solid-phase dispersion extraction was used to separated andconcentrated the hormones from feeds and antler velvet.The high-performance liquidchromatography mass spectrometry was applied to the determination of the hormones.The influence factors including dispersant type, ratio of samples to dispersant, typesand volume of elution solvent are investigated. The results indicated that theextraction efficiency of fourteen kinds of hormones were highest when the ratio ofsamples to dispersant is1:4and30mL methanol-water solution(V:V=4:1) wasselected as the elution solvent. The extraction solution was evaporated to dryness,dissolved by1.0mL of methanol, filtered through0.45μm filter and then analyzed byliquid chromatography-electrospray ionization mass spectrometry. The establishedmethod can achieve the extraction and purification of the target analyte in one step.The result indicates there are many virtues for this method, such as high purificationefficiency, less analytical time, and small amount of sample and solvent. In addition,the recoveries of the analytes range from83.40to99.17%and RSDs are lower than7.42%. The LODs are lower than7.00ng kg-1.
引文
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