A method of gradient-elution HPLC with UV detection was developed for theanalysis of nine major constituents of Salvia species, a commonly used TCM herb, namely danshensu,protocatechuic acid, protocatechualdehyde, sal...A method of gradient-elution HPLC with UV detection was developed for theanalysis of nine major constituents of Salvia species, a commonly used TCM herb, namely danshensu,protocatechuic acid, protocatechualdehyde, salviano-lic acid B, methyltanshinone, dihydrotanshinone,cryptotanshinone, tanshinoneⅠand tanshinoneⅡ_A. In the present study, a Shimadzu CLC-ODS column(150 mm x 6 mm, 5 μm) was utilized and 0.5% formic acid (A) and acetonitrile (B) were used forgradient elution at a total flow rate of 0.8 mL· min^(-1). All calibration curves showed goodlinear regression ( r > 0.999) within test ranges. Extraction was conducted by refluxing methanol(10 mL) with dried herb (0.5 g) for 1.0 h.The assay was simple, convenient and reproducible. Theproposed method was successfully applied to the determination of nine major constituents in thirteenSalvia. species and the results showed that the contents of Salvia components vary in differentspecies and origin. Tanshinone was hardly detected in S. yunnanensis and S. prionitis, thereforethey are not suitable for clinical use as Danshen.展开更多
[Objective] This study was conducted to establish a near-infrared diffuse reflectance spectroscopy of Guizhou Aspidistra plants. [Method] Twenty three batch- es of Guizhou Aspidistra plants including A. chishuiensis, ...[Objective] This study was conducted to establish a near-infrared diffuse reflectance spectroscopy of Guizhou Aspidistra plants. [Method] Twenty three batch- es of Guizhou Aspidistra plants including A. chishuiensis, A. spinula, A. Caespitosa, A. sichuanensis, A. ebianensis, A. retusa, A. guizhouensis and A. liboensis were subjected to drying, pulverization and sieving and then directly determined for near- infrared reflectance spectrums; and the plants in this genus were classified by clus- ter analysis and principal component analysis (PCA). [Result] The near-infrared re- flectance spectrums of the 23 batches of Guizhou Aspidistra plants showed very high similarity. The spectrums were processed by first derivative method, and the spectral range of 4 000-7 500 cm-1 was selected as the analytical range. Cluster analysis and PCA were employed to mass spectrum variables of plants in Aspidis- tra, fewer new variables became the linear combination of primary variables, and small differences between different varieties were enlarged, thereby facilitating intu- itive classification of plants in this genus. [Conclusion] Near-infrared diffuse re- flectance spectroscopy is nondestructive and rapid for determination of solid sam- pies, and provides a new method for the classification of Guizhou Aspidistra plants combined by information processing techniques.展开更多
Phytoremediation effectiveness and remediation costs are driving factors of this project. Full utilization of plant resources after their being used for phytoremediation is an unsolved problem. GC/MS technique was use...Phytoremediation effectiveness and remediation costs are driving factors of this project. Full utilization of plant resources after their being used for phytoremediation is an unsolved problem. GC/MS technique was used to investigate the volatiles of the flowers from Elsholtzia argyi (PFE1: Purple Flower Elsholtzia) and their variation (WFE: White Flower Elsholtzia),naturally growing in Pb/Zn mined area, and Elsholtzia argyi (PFE2: Purple Flower Elsholtzia), naturally growing in Jiuxi uncontaminated agriculture soil. Seventeen compounds constituting 86.88% of total essential oils were identified in PFE1, with 2,6-octadienoic acid,3,7-dimethyl-methyl ester being the main constituent (63.30%). Sixteen compounds accounting for 95.32% of total essential oils were identified in WFE, with caryophyllene being the main component (55.02%). Compared to PFE1, PFE2 contained lower level of 2,6-octadienoic acid,3,7-dimethyl-methyl ester (31.76%), which was the main constituent in the total essential oils of PFE2. Caryophyllene is the main ingredient of flavor. Elsholtzia ketone was identified in all the three Elsholtzia plants. It can be concluded that the selected Elsholtzia argyi plants can be exploited on their versatile uses as fragrances and antiseptics due to the perfume ingredient and antibacterial components existing in their essential oils.展开更多
The sensitive second derivative waves of Cu(Ⅱ),Pb(Ⅱ),Cd(Ⅱ),Ni(Ⅱ),Zn(Ⅱ),Fe(Ⅱ)and Mn(Ⅱ),forming in the substrate solution(pH=9.26)consisting of ammonia,ammonium chlorid,gelatin and ascorbic acid were researched.T...The sensitive second derivative waves of Cu(Ⅱ),Pb(Ⅱ),Cd(Ⅱ),Ni(Ⅱ),Zn(Ⅱ),Fe(Ⅱ)and Mn(Ⅱ),forming in the substrate solution(pH=9.26)consisting of ammonia,ammonium chlorid,gelatin and ascorbic acid were researched.The peak potentials of the polarographic waves of the seven ions are at about 0.48,0.63,0.79,1.04,1.28,1.44 and 1.60 V respectively.Combining with microwave technique,a new method for the simultaneous determination of the seven trace elements in Chinese traditional medicine was developed.The method is easy to operate,rapid,simple and convenient.When the signal-to-noise rate equals 3,the detection limits of Cu,Pb,Cd,Ni,Zn,Fe and Mn are 4.2×10 3,5.3×10 3,2.1×10 3,5.8×10 4,3.0×10 3,7.7×10 4 and 1.1×10 3 μg/mL respectively.Well linear relationships exist between the concentrations and the peak currents when Cu,Pb,Cd,Ni,Zn,Fe and Mn concentrations are within 8.5×10 3 10,9.7×10 3 10,4.5×10 3 10,1.2×10 3 10,6.4×10 3 10,1.5×10 3 10 and 2.8×10 3 10 μg/mL,respectively.The method has been used to the simultaneous determination of the seven trace elements in Salvia Miltiorrhiza Root and compound Salvia Miltiorrhiza Root injection,the relative standard deviations(RSDs)of the Cu,Pb,Cd,Ni,Zn,Fe and Mn in the two medicines are 3.9% and 5.8%,4.0% and 4.1%,4.3% and 5.7%,4.9% and 5.3%,4.4% and 4.7%,3.5% and 4.0%,0.51% and 2.8%,respectively;the comparisons of the determination results with the values obtained by the standard method indicate that the presented method has very well veracity.展开更多
AIM:To clarify the protective effect of exogenous adenosine triphosphate(ATP)on hypothermically preserved rat livers. METHODS:Establishment of continuous hypothermic machine perfusion model,detection of nucleotides in...AIM:To clarify the protective effect of exogenous adenosine triphosphate(ATP)on hypothermically preserved rat livers. METHODS:Establishment of continuous hypothermic machine perfusion model,detection of nucleotides in hepatocytes with HPLC,measurement of activities of LDH and AST in the perfusate,observation of histopathological changes in different experiment groups,and autoradiography were carried out to reveal the underlying mechanism of the protective effect of ATP. RESULTS:The intracellular levels of ATP and EC decreased rapidly after hypothermic preservation in control group,while a higher ATP and EC level,and a slower decreasing rate were observed when ATP-MgCl_2 was added to the perfusate (P<0.01).As compared with the control group,the activities of LDH and AST in the ATP-MgCl_2 group were lower(P<0.05). Furthermore,more severe hepatocyte damage and neutrophil infiltration were observed in the control group.Radioactive [α-^(32)P]ATP entered the hypothermically preserved rat hepatocytes. CONCLUSION:Exogenous ATP has a protective effect on rat livers during hypothermical preservation.However,Mg^(2+) is indispensable,addition of ATP alone produces no protective effect.The underlying mechanism may be that exogenous ATP enters the hypothermically preserved rat liver cells.展开更多
A bloom of the dinoflagellate Scrippsiella trochoidea was detected for the first time in inner Tolo Harbor,Hong Kong in 2 000. Water samples were collected at eight stations along a transect passing through a red tide...A bloom of the dinoflagellate Scrippsiella trochoidea was detected for the first time in inner Tolo Harbor,Hong Kong in 2 000. Water samples were collected at eight stations along a transect passing through a red tide patch for microscopic analysis of phytoplankton composition and high-performance liquid chromatography(HPLC) analysis of phytoplankton pigments. During the bloom,the density of dinoflagellates was 1.1×106 cells L-1 within the patch and 8.6×105 cells L-1 outside the patch where the phytoplankton community was dominated by diatoms. After the bloom the S. trochoidea began to decrease in density and was replaced by diatoms as the dominating bloom-causing organisms at all stations,and the density of dinoflagellates at most stations was less than 1.0 × 106 cells L-1. The status of S. trochoidea as the causative species of the bloom was indicated by the presence of peridinin,the marker pigment for dinoflagellates. The shift from dinoflagellates to diatoms was marked by the decline of peridinin and the prevalence of fucoxanthin. Phytoplankton pigment markers also revealed the presence of other minor phytoplankton assemblages such as cryptomonads and blue-green algal.展开更多
This paper presents the possibilities offered by fluorescence spectroscopy for the identification of vegetable oils such as soybean, sunflower, flax, walnut, corn, almond, sesame, olive and pumpkin oils. The probes un...This paper presents the possibilities offered by fluorescence spectroscopy for the identification of vegetable oils such as soybean, sunflower, flax, walnut, corn, almond, sesame, olive and pumpkin oils. The probes under study have been excited with two types of sources: a laser diode (LD) and light-emitting diodes (LEDs) emitting in the UV and in the visible range. Total luminescence spectra were recorded by measuring the emission spectra in the range 350-720 nm at excitation wavelengths from 375 to 450 nm. The excitation-emission matrices have been obtained and two basic fluorescence regions in the visible have been outlined. On this basis the fluorescence spectra of the oils have been subdivided into three categories depending on the prevalence of the fluorescence maxima. The samples show differences in their fluorescence spectra. The latter fact shows that fluorescence spectroscopy can be used for the quick identification of edible oils. The fatty acid, the tocopherol, the beta-carotene and chlorophyll contents in the analyzed oils have been studied. It is shown that some of the types of oils differ significantly from each other by the first derivatives of their fluorescence spectra. There also exist color differences between the groups of vegetable oils under study.展开更多
The increase of import/export of every kind of herbal products calls urgently for adequate controls. Analysis of herbal food supplement (botanicals) is a difficult task, like in the composition determination of a mu...The increase of import/export of every kind of herbal products calls urgently for adequate controls. Analysis of herbal food supplement (botanicals) is a difficult task, like in the composition determination of a multi-ingredient product, where several botanical drugs were used. Actually, this is an important argument in consideration of health security. The authors reported the results of an analytical approach based on HPTLC (high performance thin layer chromatography) fingerprints comparison and tailored to determine the composition of marketed multi-ingredient botanicals. The method gave positive data in case of the presence of 3-5 species, whereas difficulties were recorded when the number of plants is increased.展开更多
A method was developed for the analysis of hydroxylated brominated diphenyl ethers (OH-PBDEs) in plant samples using an ultra performance liquid chromatography-triple quadrupole mass spectrometer (UPLC-ESI-MS/MS) in n...A method was developed for the analysis of hydroxylated brominated diphenyl ethers (OH-PBDEs) in plant samples using an ultra performance liquid chromatography-triple quadrupole mass spectrometer (UPLC-ESI-MS/MS) in negative mode. Plant samples were extracted and cleaned up through florisil column, resolved on a 100 mm C18 column with linear gradient elution and detected by mass spectrometry in multiple reaction monitoring (MRM) mode. The method provided good recoveries rang- ing from 68.2% to 94.6%, relative standard deviation (RSD) in the range of 3.2% - 9.1%, and limits of quantification (LOQ) defined as the signal-to-noise ratio of 10 of 0.3-2.1 ng/g. It allowed a fast separation and sensitive quantification of the isomers and homologues of seven OH-PBDE congeners 2′-OH-BDE-3, 3′-OH-BDE-7, 4′-OH-BDE-17, 3′-OH-BDE-28, 3-OH-BDE-47, 5-OH-BDE-47 and 6-OH-BDE-47. The method was successfully applied to identify and quantify the formation of hydroxylat- ed metabolites in alfalfa exposed to BDE-209. Five OH-PBDEs were detected in plant tissues, and more congeners were found in roots than in shoots. To our knowledge, this work represents the first attempt to validate UPLC-MS/MS method to quantify OH-PBDEs in plant samples without derivatization.展开更多
Sedimentary pigments are useful proxy indicators of phytoplankton biomass, community structure, primary productivity and human influence in lacustrine and oceanic ecosystems. Pigments are relatively labile due to thei...Sedimentary pigments are useful proxy indicators of phytoplankton biomass, community structure, primary productivity and human influence in lacustrine and oceanic ecosystems. Pigments are relatively labile due to their complex chemical structures, which makes the extraction and analysis of sedimentary pigments challenging. In addition, it is important to select appropriate methods to study sedimentary pigments in regions which lack previous investigations. In this study, we adopted the L9(34) orthogonal design to develop methods of extraction and HPLC (high performance liquid chromatography) analysis of sedimentary pigments at two lakes on the Tibetan Plateau: meromictic lake-Dagze Co and dimictic lake-Jiang Co. The orthogonal design comprises 9 combinations of various parameters for extraction and HPLC analysis. The results show that the type and volume of solvent are the most important factors for pigment extraction, and the mobile phase and column selection are the most important for HPLC analysis. For the study sites, we found that the best methods to extract sedimentary pigments are as follows: the use of a mixture of acetone:methanol:water (80: 15:5, v:v:v) as the extraction solvent; sol- vent/sample ratio of 10 mL/g; sonication for 30 s and standing extraction for 6 h. The best methods for HPLC analysis are as follows: Zorbax Eclipse plus C8 column with mobile phase A, methanol:acetonitrile:0.25 M aqueous pyridine (50: 25:25, v : v : v) and mobile phase B, methanol: acetonitrile: acetone (20: 60: 20, v: v: v); pH of mobile phase A adjusted to 6 with acetic acid; and HPLC column temperature maintained at 40~C. The study provides an experimental basis for future investigations of past changes in primary productivity and the response of lake ecosystems to climate change and human activities on the Tibetan Plateau.展开更多
文摘A method of gradient-elution HPLC with UV detection was developed for theanalysis of nine major constituents of Salvia species, a commonly used TCM herb, namely danshensu,protocatechuic acid, protocatechualdehyde, salviano-lic acid B, methyltanshinone, dihydrotanshinone,cryptotanshinone, tanshinoneⅠand tanshinoneⅡ_A. In the present study, a Shimadzu CLC-ODS column(150 mm x 6 mm, 5 μm) was utilized and 0.5% formic acid (A) and acetonitrile (B) were used forgradient elution at a total flow rate of 0.8 mL· min^(-1). All calibration curves showed goodlinear regression ( r > 0.999) within test ranges. Extraction was conducted by refluxing methanol(10 mL) with dried herb (0.5 g) for 1.0 h.The assay was simple, convenient and reproducible. Theproposed method was successfully applied to the determination of nine major constituents in thirteenSalvia. species and the results showed that the contents of Salvia components vary in differentspecies and origin. Tanshinone was hardly detected in S. yunnanensis and S. prionitis, thereforethey are not suitable for clinical use as Danshen.
基金Supported by National Natural Science Foundation of China(81360623)~~
文摘[Objective] This study was conducted to establish a near-infrared diffuse reflectance spectroscopy of Guizhou Aspidistra plants. [Method] Twenty three batch- es of Guizhou Aspidistra plants including A. chishuiensis, A. spinula, A. Caespitosa, A. sichuanensis, A. ebianensis, A. retusa, A. guizhouensis and A. liboensis were subjected to drying, pulverization and sieving and then directly determined for near- infrared reflectance spectrums; and the plants in this genus were classified by clus- ter analysis and principal component analysis (PCA). [Result] The near-infrared re- flectance spectrums of the 23 batches of Guizhou Aspidistra plants showed very high similarity. The spectrums were processed by first derivative method, and the spectral range of 4 000-7 500 cm-1 was selected as the analytical range. Cluster analysis and PCA were employed to mass spectrum variables of plants in Aspidis- tra, fewer new variables became the linear combination of primary variables, and small differences between different varieties were enlarged, thereby facilitating intu- itive classification of plants in this genus. [Conclusion] Near-infrared diffuse re- flectance spectroscopy is nondestructive and rapid for determination of solid sam- pies, and provides a new method for the classification of Guizhou Aspidistra plants combined by information processing techniques.
文摘Phytoremediation effectiveness and remediation costs are driving factors of this project. Full utilization of plant resources after their being used for phytoremediation is an unsolved problem. GC/MS technique was used to investigate the volatiles of the flowers from Elsholtzia argyi (PFE1: Purple Flower Elsholtzia) and their variation (WFE: White Flower Elsholtzia),naturally growing in Pb/Zn mined area, and Elsholtzia argyi (PFE2: Purple Flower Elsholtzia), naturally growing in Jiuxi uncontaminated agriculture soil. Seventeen compounds constituting 86.88% of total essential oils were identified in PFE1, with 2,6-octadienoic acid,3,7-dimethyl-methyl ester being the main constituent (63.30%). Sixteen compounds accounting for 95.32% of total essential oils were identified in WFE, with caryophyllene being the main component (55.02%). Compared to PFE1, PFE2 contained lower level of 2,6-octadienoic acid,3,7-dimethyl-methyl ester (31.76%), which was the main constituent in the total essential oils of PFE2. Caryophyllene is the main ingredient of flavor. Elsholtzia ketone was identified in all the three Elsholtzia plants. It can be concluded that the selected Elsholtzia argyi plants can be exploited on their versatile uses as fragrances and antiseptics due to the perfume ingredient and antibacterial components existing in their essential oils.
基金Proejcr(20235020) supported by the National Natural Science Foundation of China
文摘The sensitive second derivative waves of Cu(Ⅱ),Pb(Ⅱ),Cd(Ⅱ),Ni(Ⅱ),Zn(Ⅱ),Fe(Ⅱ)and Mn(Ⅱ),forming in the substrate solution(pH=9.26)consisting of ammonia,ammonium chlorid,gelatin and ascorbic acid were researched.The peak potentials of the polarographic waves of the seven ions are at about 0.48,0.63,0.79,1.04,1.28,1.44 and 1.60 V respectively.Combining with microwave technique,a new method for the simultaneous determination of the seven trace elements in Chinese traditional medicine was developed.The method is easy to operate,rapid,simple and convenient.When the signal-to-noise rate equals 3,the detection limits of Cu,Pb,Cd,Ni,Zn,Fe and Mn are 4.2×10 3,5.3×10 3,2.1×10 3,5.8×10 4,3.0×10 3,7.7×10 4 and 1.1×10 3 μg/mL respectively.Well linear relationships exist between the concentrations and the peak currents when Cu,Pb,Cd,Ni,Zn,Fe and Mn concentrations are within 8.5×10 3 10,9.7×10 3 10,4.5×10 3 10,1.2×10 3 10,6.4×10 3 10,1.5×10 3 10 and 2.8×10 3 10 μg/mL,respectively.The method has been used to the simultaneous determination of the seven trace elements in Salvia Miltiorrhiza Root and compound Salvia Miltiorrhiza Root injection,the relative standard deviations(RSDs)of the Cu,Pb,Cd,Ni,Zn,Fe and Mn in the two medicines are 3.9% and 5.8%,4.0% and 4.1%,4.3% and 5.7%,4.9% and 5.3%,4.4% and 4.7%,3.5% and 4.0%,0.51% and 2.8%,respectively;the comparisons of the determination results with the values obtained by the standard method indicate that the presented method has very well veracity.
文摘AIM:To clarify the protective effect of exogenous adenosine triphosphate(ATP)on hypothermically preserved rat livers. METHODS:Establishment of continuous hypothermic machine perfusion model,detection of nucleotides in hepatocytes with HPLC,measurement of activities of LDH and AST in the perfusate,observation of histopathological changes in different experiment groups,and autoradiography were carried out to reveal the underlying mechanism of the protective effect of ATP. RESULTS:The intracellular levels of ATP and EC decreased rapidly after hypothermic preservation in control group,while a higher ATP and EC level,and a slower decreasing rate were observed when ATP-MgCl_2 was added to the perfusate (P<0.01).As compared with the control group,the activities of LDH and AST in the ATP-MgCl_2 group were lower(P<0.05). Furthermore,more severe hepatocyte damage and neutrophil infiltration were observed in the control group.Radioactive [α-^(32)P]ATP entered the hypothermically preserved rat hepatocytes. CONCLUSION:Exogenous ATP has a protective effect on rat livers during hypothermical preservation.However,Mg^(2+) is indispensable,addition of ATP alone produces no protective effect.The underlying mechanism may be that exogenous ATP enters the hypothermically preserved rat liver cells.
基金supported by a Direct Grant for Research from The Chinese University of Hong Kong to Wong C. K.
文摘A bloom of the dinoflagellate Scrippsiella trochoidea was detected for the first time in inner Tolo Harbor,Hong Kong in 2 000. Water samples were collected at eight stations along a transect passing through a red tide patch for microscopic analysis of phytoplankton composition and high-performance liquid chromatography(HPLC) analysis of phytoplankton pigments. During the bloom,the density of dinoflagellates was 1.1×106 cells L-1 within the patch and 8.6×105 cells L-1 outside the patch where the phytoplankton community was dominated by diatoms. After the bloom the S. trochoidea began to decrease in density and was replaced by diatoms as the dominating bloom-causing organisms at all stations,and the density of dinoflagellates at most stations was less than 1.0 × 106 cells L-1. The status of S. trochoidea as the causative species of the bloom was indicated by the presence of peridinin,the marker pigment for dinoflagellates. The shift from dinoflagellates to diatoms was marked by the decline of peridinin and the prevalence of fucoxanthin. Phytoplankton pigment markers also revealed the presence of other minor phytoplankton assemblages such as cryptomonads and blue-green algal.
文摘This paper presents the possibilities offered by fluorescence spectroscopy for the identification of vegetable oils such as soybean, sunflower, flax, walnut, corn, almond, sesame, olive and pumpkin oils. The probes under study have been excited with two types of sources: a laser diode (LD) and light-emitting diodes (LEDs) emitting in the UV and in the visible range. Total luminescence spectra were recorded by measuring the emission spectra in the range 350-720 nm at excitation wavelengths from 375 to 450 nm. The excitation-emission matrices have been obtained and two basic fluorescence regions in the visible have been outlined. On this basis the fluorescence spectra of the oils have been subdivided into three categories depending on the prevalence of the fluorescence maxima. The samples show differences in their fluorescence spectra. The latter fact shows that fluorescence spectroscopy can be used for the quick identification of edible oils. The fatty acid, the tocopherol, the beta-carotene and chlorophyll contents in the analyzed oils have been studied. It is shown that some of the types of oils differ significantly from each other by the first derivatives of their fluorescence spectra. There also exist color differences between the groups of vegetable oils under study.
文摘The increase of import/export of every kind of herbal products calls urgently for adequate controls. Analysis of herbal food supplement (botanicals) is a difficult task, like in the composition determination of a multi-ingredient product, where several botanical drugs were used. Actually, this is an important argument in consideration of health security. The authors reported the results of an analytical approach based on HPTLC (high performance thin layer chromatography) fingerprints comparison and tailored to determine the composition of marketed multi-ingredient botanicals. The method gave positive data in case of the presence of 3-5 species, whereas difficulties were recorded when the number of plants is increased.
基金funded by the National Natural Science Foundation of China (40730740 & 20921063)the National Basic Research Program of China (2009CB421603)
文摘A method was developed for the analysis of hydroxylated brominated diphenyl ethers (OH-PBDEs) in plant samples using an ultra performance liquid chromatography-triple quadrupole mass spectrometer (UPLC-ESI-MS/MS) in negative mode. Plant samples were extracted and cleaned up through florisil column, resolved on a 100 mm C18 column with linear gradient elution and detected by mass spectrometry in multiple reaction monitoring (MRM) mode. The method provided good recoveries rang- ing from 68.2% to 94.6%, relative standard deviation (RSD) in the range of 3.2% - 9.1%, and limits of quantification (LOQ) defined as the signal-to-noise ratio of 10 of 0.3-2.1 ng/g. It allowed a fast separation and sensitive quantification of the isomers and homologues of seven OH-PBDE congeners 2′-OH-BDE-3, 3′-OH-BDE-7, 4′-OH-BDE-17, 3′-OH-BDE-28, 3-OH-BDE-47, 5-OH-BDE-47 and 6-OH-BDE-47. The method was successfully applied to identify and quantify the formation of hydroxylat- ed metabolites in alfalfa exposed to BDE-209. Five OH-PBDEs were detected in plant tissues, and more congeners were found in roots than in shoots. To our knowledge, this work represents the first attempt to validate UPLC-MS/MS method to quantify OH-PBDEs in plant samples without derivatization.
基金supported by National Key Basic Research Programs of China (Grant No. 2012CB956100)the National Natural Science Foundation of China (Grant Nos. 41072120 & 41321061)
文摘Sedimentary pigments are useful proxy indicators of phytoplankton biomass, community structure, primary productivity and human influence in lacustrine and oceanic ecosystems. Pigments are relatively labile due to their complex chemical structures, which makes the extraction and analysis of sedimentary pigments challenging. In addition, it is important to select appropriate methods to study sedimentary pigments in regions which lack previous investigations. In this study, we adopted the L9(34) orthogonal design to develop methods of extraction and HPLC (high performance liquid chromatography) analysis of sedimentary pigments at two lakes on the Tibetan Plateau: meromictic lake-Dagze Co and dimictic lake-Jiang Co. The orthogonal design comprises 9 combinations of various parameters for extraction and HPLC analysis. The results show that the type and volume of solvent are the most important factors for pigment extraction, and the mobile phase and column selection are the most important for HPLC analysis. For the study sites, we found that the best methods to extract sedimentary pigments are as follows: the use of a mixture of acetone:methanol:water (80: 15:5, v:v:v) as the extraction solvent; sol- vent/sample ratio of 10 mL/g; sonication for 30 s and standing extraction for 6 h. The best methods for HPLC analysis are as follows: Zorbax Eclipse plus C8 column with mobile phase A, methanol:acetonitrile:0.25 M aqueous pyridine (50: 25:25, v : v : v) and mobile phase B, methanol: acetonitrile: acetone (20: 60: 20, v: v: v); pH of mobile phase A adjusted to 6 with acetic acid; and HPLC column temperature maintained at 40~C. The study provides an experimental basis for future investigations of past changes in primary productivity and the response of lake ecosystems to climate change and human activities on the Tibetan Plateau.