A simple and accurate high-performance liquid chromatography（HPLC）coupled with diode array detector（DAD）and evaporative light scattering detector（ELSD）was established for the determination of six bioactive compo...A simple and accurate high-performance liquid chromatography（HPLC）coupled with diode array detector（DAD）and evaporative light scattering detector（ELSD）was established for the determination of six bioactive compounds in Zhenqi Fuzheng preparation（ZFP）.The monitoring wavelengths were 254,275 and 328 nm.Under the optimum conditions,good separation was achieved,and the assay was fully validated in respect of precision,repeatability and accuracy.The proposed method was successfully applied to quantify the six ingredients in 31 batches of ZFP samples and evaluate the variation by hierarchical cluster analysis（HCA）,which demonstrated significant variations on the content of these compounds in the samples from different manufacturers with different preparation procedures.The developed HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of this preparation.展开更多
In this study, an optimized high performance liquid chromatography-fluorescence detector (HPLC-FL) method for the determination of benzo[a]pyrene in edible oil was established. HPLC was performed with Thermo Fisher Sc...In this study, an optimized high performance liquid chromatography-fluorescence detector (HPLC-FL) method for the determination of benzo[a]pyrene in edible oil was established. HPLC was performed with Thermo Fisher Scientific C18 column (250 mm×4.6 mm, 5 μm) as the chromatographic column and acetonitrile and water as the mobile phase, and the excitation wavelength and emission wavelength of fluorescence detector were 286 and 430 nm, respectively. The response was high, and the linear range was 0.5-10.0 ng/ml. The lowest limit of detection was 0.11 ng/ml, and the average recovery was 92.5%. This method is suitable for quantitative analysis of benzo[a]pyrene content in edible oil.展开更多
[Objective]The paper was to establish a method for determining AF and AFG in red ginseng.[Method]A new simple,rapid and sensitive method for simultaneous determination of two amadori compounds,arginyl-fructose(AF)and ...[Objective]The paper was to establish a method for determining AF and AFG in red ginseng.[Method]A new simple,rapid and sensitive method for simultaneous determination of two amadori compounds,arginyl-fructose(AF)and arginyl-fructosyl-glucose(AFG),in extracts of three kinds of ginseng preparations was developed and validated using high performance liquid chromatography with evaporative light scattering detector(HPLC-ELSD).Two target analytes were efficiently separated by Prevail CTM18 column(4.6 mm×250 mm,5μm)at the flow rate of 0.8 mL/min within 15 min of single chromatographic run.[Result]Under optimized conditions,the detection limits were 0.015 and 0.02 mg/mL for AF and AFG,respectively.Calibration curves of peak area for two analytes were linear over three orders of magnitude with the correlation coefficients greater than 0.999.The average recoveries,precision,reproducibility and stability for two analytes(AF and AFG)were 99.5% and 100.9%,0.43% and 0.47%,0.46% and 0.43%,0.41% and 0.49%,respectively.[Conclusion]This method was successfully applied for quantifying AF and AFG in red ginseng and the method was efficient,sensitive and accurate.展开更多
As a highly sensitive and stable detector,refractive index detector is usually used for quantitative detection of substances such as polymer,sugar and organic acid. The research reviewed the application of HPLC-RID in...As a highly sensitive and stable detector,refractive index detector is usually used for quantitative detection of substances such as polymer,sugar and organic acid. The research reviewed the application of HPLC-RID in the fields of quantitative determination of medicine and food,in order to lay a foundation for wider use of RID.展开更多
A novel method for the determination of five carbamate pesticides （metolcarb, carbofuran, carbaryl, isoprocard and diethofencard） in water samples was developed by dispersive liquid-liquid microextraction （DLLME） ...A novel method for the determination of five carbamate pesticides （metolcarb, carbofuran, carbaryl, isoprocard and diethofencard） in water samples was developed by dispersive liquid-liquid microextraction （DLLME） coupled with high performance liquid chromatography-diode array detector （HPLC-DAD）. Some experimental parameters that influence the extraction efficiency were studied and optimized to obtain the best extraction results. Under the optimum conditions for the method, the calibration curve was linear in the concentration range from 5 to 1000 ng mL^-1 for all the five carbamate pesticides, with the correlation coefficients （r^2） varying from 0.9984 to 0.9994. Good enrichment factors were achieved ranging from 80 to 177- fold, depending on the compound. The limits of detection （LODs） （S/N = 3） were ranged from 0.1 to 0.5 ng mL^-1. The method has been successfully applied to the analysis of the pesticide residues in environmental water samples.展开更多
To establish a method for determining five saponins(notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ammonium glycyrrhizinate) in Glycyrrhizae, Notoginseng and Ginseng, the high performance liq...To establish a method for determining five saponins(notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ammonium glycyrrhizinate) in Glycyrrhizae, Notoginseng and Ginseng, the high performance liquid chromatography with diode array detector(HPLC-DAD) method was applied to an Inertsil ODS-SP column(4.6 mm×250 mm, 5 μm) with a mobile phase consisting of acetonitrile-0.05% phosphoric acid in a gradient elution manner. The flow rate was 1.0 mL/min. The column temperature was 30 ℃ and the detection wavelengths were 203 nm and 237 nm, respectively. The linear ranges were 0.700,0—7.000,0 μg for R1(r=1.000,0), 0.751,1— 7.511,4 μg for Rg1(r=1.000,0), 0.677,2—6.771,6 μg for Re(r=1.000,0), 0.733,9—7.339,1 μg for Rb1(r= 1.000,0), and 0.540,0—5.399,8 μg for ammonium glycyrrhizinate(r=0.999,9), respectively. In addition, their average recoveries were 100.28%, 105.83%, 104.09%, 99.36% and 98.54%, respectively. The relative standard deviations(RSDs) of precision, reproducibility and recovery were all less than 1.5%. The results indicate that the method is simple, accurate and reproducible so that it can be used for the simultaneous determination of the five saponins in Chinese patent medicines containing the three kinds of herbs.展开更多
A simple and direct method without a deriva- tion step for routine analysis of tobramycin has been developed. This method used reversed-phase ion-pair high performance liquid chromatography （HPLC） with a refractive ...A simple and direct method without a deriva- tion step for routine analysis of tobramycin has been developed. This method used reversed-phase ion-pair high performance liquid chromatography （HPLC） with a refractive index （RI） detector and a C18 column which is stable at pH above 1.00. The presence of 4.50mg.mL ] trifluoroacetic acid （TFA） in the mobile phase improved the protonation of tobramycin and the formation of ionpairs, and thus reduced its hydrophility. This unique separation-detection combination showed good linearity with correlation coefficients 0.9996 in the concentration range of 0.25-2.50mg.mL 1. The quantitation limit and detection limit were determined to be 0.23 mg.mL ~ and 0.071 mg. mL ~, respectively. Tobramycin was recovered in 98.00%, 98.84% and 99.64% for tobramycin solutions at concentrations of 2.25 mg.mL^-1, 1.50mg.mL 1 and 0.75 mg.mL ＇, respectively. The relative standard deviations for six spiked samples ranged from 0.20% to 2.40%, indicating a good reproducibility of this method.展开更多
Leaves of Ziziphus jujuba Mill.（Z. jujuba） were used as a folk medicine to treat children suffering from typhoid fever, furuncle and ecthyma in China. The present study was to establish a high performance liquid chr...Leaves of Ziziphus jujuba Mill.（Z. jujuba） were used as a folk medicine to treat children suffering from typhoid fever, furuncle and ecthyma in China. The present study was to establish a high performance liquid chroma- tography-diode array detector（HPLC-DAD） method for quality control of Z. jujuba leaves. The validated method was applied to the simultaneous characterization and quantification of sixteen main constituents in thirty samples, which comprised the whole life stage of Z. ]ujuba leaves from six cultivars in Yulin, Shannxi Province, China. HPLC fin- gerprint file of Z. jujuba leaves was set up and the results indicate that the major constituents of Z. jujuba leaves are （-）-catechin（1）, quercetin-3-O-robinobioside（3）, rutin（4） and quercetin-3-O-a-L-arabinosyl-（1---~2）-a-L-rhamnoside（6） with the total contents of the nine flavonoids in respective batch ranging from 18.52 mg/g to 39.51 mg/g. In addition, the contents of compounds depend on both the season and the cultivar. During ripening of Z. jujuba leaves, flavo- noids of all the cultivars present a similar trend： initially decrease from 25th, Jun. to 5th, Aug., 2015, and then in- crease for a period of time, finally slightly fluctuate on 5th Oct. The highest contents of total flavonoids were regis- tered on 25th Jun., 2015. Different cultivars have 50%--90% variation on the content for the three classes of com- pounds. Taken together, the results demonstrate that Z. jujuba leaves have great potential to be a new health-promoting resource based on flavonoids and the best sampling time of them is in June.展开更多
Microwave-assisted extraction(MAE)was used for extraction of effective components of sarcandra glabra(Thunb.),and then chromatographic fingerprint of sarcandra glabra(Thunb.)was studied by high performance liquid chro...Microwave-assisted extraction(MAE)was used for extraction of effective components of sarcandra glabra(Thunb.),and then chromatographic fingerprint of sarcandra glabra(Thunb.)was studied by high performance liquid chromatography/diode array detector(HPLC/DAD).The conditions of MAE were optimized by an orthogonal experiment,and then the authentication and validation of the chromatographic fingerprint were conducted.Nine peaks were identified as common peaks in the fingerprint chromatograms,and isofraxidin was considered as a reference compound and quantified.Relative standard deviations of retention time and peak area of each component were less than 3% and 8%,respectively.Similarity and difference analysis were conducted by use of PCA and relation coefficient.Twenty batches of sarcandra glabra(Thunb.)samples from two different producing areas could be classified into two different groups in the PCA model.The results showed that MAE-HPLC/DAD method was simple,efficient and stable for the study of complex chromatographic fingerprint of sarcandra glabra(Thunb.),which could provide more reliable and precise information for quality evaluation.展开更多
Egg yolk phosphatidylcholine(EYPC) is being widely used in food and pharmaceutical industries nowadays owing to its surface activity,pharmaceutical usefulness,and so on.Common determination methods of phospholipids we...Egg yolk phosphatidylcholine(EYPC) is being widely used in food and pharmaceutical industries nowadays owing to its surface activity,pharmaceutical usefulness,and so on.Common determination methods of phospholipids were based on the American Oil Chemists' Society(AOCS) Official Method Ja7b-91,in which n-hexane/2-propanol/acetate buffer was used as the mobile phase.In order to achieve desired results,gradient elu-tion or buffer solution was used,which made the detection process more complicated.Moreover,water or buffer solution could affect the silica gel column both on its lifespan and the separation efficiency significantly.In this study,different mobile phase and detector were used to simplify EYPC analyzing process instead of using water within the mobile phase.The optimized HPLC operating conditions are as follows:pure methanol as a mobile phase,flow rate of 1.0 ml·min-1,silica gel column(250 mm×4.6 mm,5 μm,Inertsil GLTM),column temperature 30 ℃ and low temperature evaporative light scattering detector(40 ℃,0.35 MPa) as used.Under this optimal condition,the linear relative coefficient of the standard curve is 0.998 and the recovery was in the range of 96.83%-101.58% with a relative standard deviation of 1.79%(n=6).展开更多
文摘A simple and accurate high-performance liquid chromatography（HPLC）coupled with diode array detector（DAD）and evaporative light scattering detector（ELSD）was established for the determination of six bioactive compounds in Zhenqi Fuzheng preparation（ZFP）.The monitoring wavelengths were 254,275 and 328 nm.Under the optimum conditions,good separation was achieved,and the assay was fully validated in respect of precision,repeatability and accuracy.The proposed method was successfully applied to quantify the six ingredients in 31 batches of ZFP samples and evaluate the variation by hierarchical cluster analysis（HCA）,which demonstrated significant variations on the content of these compounds in the samples from different manufacturers with different preparation procedures.The developed HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of this preparation.
文摘In this study, an optimized high performance liquid chromatography-fluorescence detector (HPLC-FL) method for the determination of benzo[a]pyrene in edible oil was established. HPLC was performed with Thermo Fisher Scientific C18 column (250 mm×4.6 mm, 5 μm) as the chromatographic column and acetonitrile and water as the mobile phase, and the excitation wavelength and emission wavelength of fluorescence detector were 286 and 430 nm, respectively. The response was high, and the linear range was 0.5-10.0 ng/ml. The lowest limit of detection was 0.11 ng/ml, and the average recovery was 92.5%. This method is suitable for quantitative analysis of benzo[a]pyrene content in edible oil.
文摘[Objective]The paper was to establish a method for determining AF and AFG in red ginseng.[Method]A new simple,rapid and sensitive method for simultaneous determination of two amadori compounds,arginyl-fructose(AF)and arginyl-fructosyl-glucose(AFG),in extracts of three kinds of ginseng preparations was developed and validated using high performance liquid chromatography with evaporative light scattering detector(HPLC-ELSD).Two target analytes were efficiently separated by Prevail CTM18 column(4.6 mm×250 mm,5μm)at the flow rate of 0.8 mL/min within 15 min of single chromatographic run.[Result]Under optimized conditions,the detection limits were 0.015 and 0.02 mg/mL for AF and AFG,respectively.Calibration curves of peak area for two analytes were linear over three orders of magnitude with the correlation coefficients greater than 0.999.The average recoveries,precision,reproducibility and stability for two analytes(AF and AFG)were 99.5% and 100.9%,0.43% and 0.47%,0.46% and 0.43%,0.41% and 0.49%,respectively.[Conclusion]This method was successfully applied for quantifying AF and AFG in red ginseng and the method was efficient,sensitive and accurate.
文摘As a highly sensitive and stable detector,refractive index detector is usually used for quantitative detection of substances such as polymer,sugar and organic acid. The research reviewed the application of HPLC-RID in the fields of quantitative determination of medicine and food,in order to lay a foundation for wider use of RID.
基金supported both by the Natural Science Foundations of Hebei(No.B2008000210)the Scientific Research Foundation of Agricultural University of Hebei.
文摘A novel method for the determination of five carbamate pesticides （metolcarb, carbofuran, carbaryl, isoprocard and diethofencard） in water samples was developed by dispersive liquid-liquid microextraction （DLLME） coupled with high performance liquid chromatography-diode array detector （HPLC-DAD）. Some experimental parameters that influence the extraction efficiency were studied and optimized to obtain the best extraction results. Under the optimum conditions for the method, the calibration curve was linear in the concentration range from 5 to 1000 ng mL^-1 for all the five carbamate pesticides, with the correlation coefficients （r^2） varying from 0.9984 to 0.9994. Good enrichment factors were achieved ranging from 80 to 177- fold, depending on the compound. The limits of detection （LODs） （S/N = 3） were ranged from 0.1 to 0.5 ng mL^-1. The method has been successfully applied to the analysis of the pesticide residues in environmental water samples.
基金Supported by Plan Issue of Shanghai Science &Technology Committee(No.13401901100)
文摘To establish a method for determining five saponins(notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ammonium glycyrrhizinate) in Glycyrrhizae, Notoginseng and Ginseng, the high performance liquid chromatography with diode array detector(HPLC-DAD) method was applied to an Inertsil ODS-SP column(4.6 mm×250 mm, 5 μm) with a mobile phase consisting of acetonitrile-0.05% phosphoric acid in a gradient elution manner. The flow rate was 1.0 mL/min. The column temperature was 30 ℃ and the detection wavelengths were 203 nm and 237 nm, respectively. The linear ranges were 0.700,0—7.000,0 μg for R1(r=1.000,0), 0.751,1— 7.511,4 μg for Rg1(r=1.000,0), 0.677,2—6.771,6 μg for Re(r=1.000,0), 0.733,9—7.339,1 μg for Rb1(r= 1.000,0), and 0.540,0—5.399,8 μg for ammonium glycyrrhizinate(r=0.999,9), respectively. In addition, their average recoveries were 100.28%, 105.83%, 104.09%, 99.36% and 98.54%, respectively. The relative standard deviations(RSDs) of precision, reproducibility and recovery were all less than 1.5%. The results indicate that the method is simple, accurate and reproducible so that it can be used for the simultaneous determination of the five saponins in Chinese patent medicines containing the three kinds of herbs.
文摘A simple and direct method without a deriva- tion step for routine analysis of tobramycin has been developed. This method used reversed-phase ion-pair high performance liquid chromatography （HPLC） with a refractive index （RI） detector and a C18 column which is stable at pH above 1.00. The presence of 4.50mg.mL ] trifluoroacetic acid （TFA） in the mobile phase improved the protonation of tobramycin and the formation of ionpairs, and thus reduced its hydrophility. This unique separation-detection combination showed good linearity with correlation coefficients 0.9996 in the concentration range of 0.25-2.50mg.mL 1. The quantitation limit and detection limit were determined to be 0.23 mg.mL ~ and 0.071 mg. mL ~, respectively. Tobramycin was recovered in 98.00%, 98.84% and 99.64% for tobramycin solutions at concentrations of 2.25 mg.mL^-1, 1.50mg.mL 1 and 0.75 mg.mL ＇, respectively. The relative standard deviations for six spiked samples ranged from 0.20% to 2.40%, indicating a good reproducibility of this method.
文摘Leaves of Ziziphus jujuba Mill.（Z. jujuba） were used as a folk medicine to treat children suffering from typhoid fever, furuncle and ecthyma in China. The present study was to establish a high performance liquid chroma- tography-diode array detector（HPLC-DAD） method for quality control of Z. jujuba leaves. The validated method was applied to the simultaneous characterization and quantification of sixteen main constituents in thirty samples, which comprised the whole life stage of Z. ]ujuba leaves from six cultivars in Yulin, Shannxi Province, China. HPLC fin- gerprint file of Z. jujuba leaves was set up and the results indicate that the major constituents of Z. jujuba leaves are （-）-catechin（1）, quercetin-3-O-robinobioside（3）, rutin（4） and quercetin-3-O-a-L-arabinosyl-（1---~2）-a-L-rhamnoside（6） with the total contents of the nine flavonoids in respective batch ranging from 18.52 mg/g to 39.51 mg/g. In addition, the contents of compounds depend on both the season and the cultivar. During ripening of Z. jujuba leaves, flavo- noids of all the cultivars present a similar trend： initially decrease from 25th, Jun. to 5th, Aug., 2015, and then in- crease for a period of time, finally slightly fluctuate on 5th Oct. The highest contents of total flavonoids were regis- tered on 25th Jun., 2015. Different cultivars have 50%--90% variation on the content for the three classes of com- pounds. Taken together, the results demonstrate that Z. jujuba leaves have great potential to be a new health-promoting resource based on flavonoids and the best sampling time of them is in June.
基金supported the National Natural Science Foundation of China(Nos.20375050 and 20905080)National Key Technologies R&D Program of the 11th-five-year Plan(No.2006BAK03A08)Guangdong Provincial Department of Science and Technology(No.2009B010900021)
文摘Microwave-assisted extraction(MAE)was used for extraction of effective components of sarcandra glabra(Thunb.),and then chromatographic fingerprint of sarcandra glabra(Thunb.)was studied by high performance liquid chromatography/diode array detector(HPLC/DAD).The conditions of MAE were optimized by an orthogonal experiment,and then the authentication and validation of the chromatographic fingerprint were conducted.Nine peaks were identified as common peaks in the fingerprint chromatograms,and isofraxidin was considered as a reference compound and quantified.Relative standard deviations of retention time and peak area of each component were less than 3% and 8%,respectively.Similarity and difference analysis were conducted by use of PCA and relation coefficient.Twenty batches of sarcandra glabra(Thunb.)samples from two different producing areas could be classified into two different groups in the PCA model.The results showed that MAE-HPLC/DAD method was simple,efficient and stable for the study of complex chromatographic fingerprint of sarcandra glabra(Thunb.),which could provide more reliable and precise information for quality evaluation.
文摘Egg yolk phosphatidylcholine(EYPC) is being widely used in food and pharmaceutical industries nowadays owing to its surface activity,pharmaceutical usefulness,and so on.Common determination methods of phospholipids were based on the American Oil Chemists' Society(AOCS) Official Method Ja7b-91,in which n-hexane/2-propanol/acetate buffer was used as the mobile phase.In order to achieve desired results,gradient elu-tion or buffer solution was used,which made the detection process more complicated.Moreover,water or buffer solution could affect the silica gel column both on its lifespan and the separation efficiency significantly.In this study,different mobile phase and detector were used to simplify EYPC analyzing process instead of using water within the mobile phase.The optimized HPLC operating conditions are as follows:pure methanol as a mobile phase,flow rate of 1.0 ml·min-1,silica gel column(250 mm×4.6 mm,5 μm,Inertsil GLTM),column temperature 30 ℃ and low temperature evaporative light scattering detector(40 ℃,0.35 MPa) as used.Under this optimal condition,the linear relative coefficient of the standard curve is 0.998 and the recovery was in the range of 96.83%-101.58% with a relative standard deviation of 1.79%(n=6).
