Some natural products, such as traditional Chinese medicines（TCMs）, contain compounds with anticancer activity and have attracted a great interest in recent years as alternative anticancer therapies. A quick and con...Some natural products, such as traditional Chinese medicines（TCMs）, contain compounds with anticancer activity and have attracted a great interest in recent years as alternative anticancer therapies. A quick and convenient assay for screening antimicrotubule compounds in which in vitro microdialysis/high-performance liquid chromatography （HPLC） is used to monitor the binding of the compounds extracted from TCM Taxus cuspidata Siebold ＆ Zucc（Taxus） to microtubules is reported. It was observed that the extract of Taxus contains at least five compounds which have affinity interaction with microtubules by biological fingerprinting analysis, and they were identified as the taxoids of taxol, baccatin III, 10-deacetylbaccatin Ⅲ（10-DAB）, cephalomannine and 7-epi-10-deacetyltaxol （7-epi-10-DAT） based on the comparison of their high-performance liquid chromatographic/mass spectrometric and UV spectra with those of the standard samples, both assembly-promoting and disassembly-inhibiting characteristics of those compounds were evaluated. It was observed that baccatin Ⅲ and 10-DAB bound to microtubules and the binding degrees were influenced by GTP. Competitive binding behavior of taxol with other four taxoids to microtubules was also investigated.展开更多
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
Objective:Belamcandae Rhizoma and Iridis Tectori Rhizoma are easily confused with each other.The main objective of this study is to distinguish them using chemical analysis.Materials and Methods:Thin-layer chromatogra...Objective:Belamcandae Rhizoma and Iridis Tectori Rhizoma are easily confused with each other.The main objective of this study is to distinguish them using chemical analysis.Materials and Methods:Thin-layer chromatography(TLC)and high-performance liquid chromatography(HPLC)fingerprint methods were established to compare the chemical profile,while HPLC quantitation was used to determine the contents of three isoflavones in thirty batches of Belamcandae Rhizoma and Iridis Tectori Rhizoma samples.Results:The two herbs could be distinguished by TLC using acetic acid-n hexane-ethyl acetate(1:90:80 v/v/v)as the mobile phase,according to the fluorescent band under 366 nm at R_(f) 0.2.In total,12 compounds were identified in the 24-min HPLC fingerprint.The similarity coefficient between the two herbs was 0.54±0.01.Mangiferin(1),tectoridin(2),iridin(3),irigenin(5),irisflorentin(6),and iristectorin A(9)were the main peaks in Belamcandae Rhizoma,while tectoridin(2)and tectorigenin(4)were the major peaks in Iridis Tectori Rhizoma.The contents of 2 in Iridis Tectori Rhizoma(2.50±0.20%)were 8.93 times higher than that of Belamcandae Rhizoma(0.28±0.08%),while the ones of 5 and 6 were slightly lower in Iridis Tectori Rhizoma.Conclusions:The study established fast and effective methods to distinguish Belamcandae Rhizoma from Iridis Tectori Rhizoma.展开更多
Objective:In this study,a comprehensive and effective quality method for evaluating the efficacy of ShuXueNing injection(SXNI)was developed.Materials and Methods:Quantitative high-performance liquid chromatography fin...Objective:In this study,a comprehensive and effective quality method for evaluating the efficacy of ShuXueNing injection(SXNI)was developed.Materials and Methods:Quantitative high-performance liquid chromatography fingerprint,the quantitative analysis of multicomponents by a single marker(QAMS)method,hierarchical cluster analysis(HCA),and orthogonal partial least squares discrimination analysis(OPLS-DA)were used to distinguish 53 batches of SXNI samples from 7 manufacturers.Results:A total of 53 batches of samples were analyzed to establish antithesis fingerprint of SXNI,and 12 peaks of the common model were collected and used for the similarity analysis.Meanwhile,six index flavonoid components were determined by the QAMS method,using rutin as internal reference substance.The accuracy of the QAMS method was confirmed by investigating the relative deviation between the QAMS method and the traditional external standard method.The results demonstrated that there was no significant difference(RE<1%),suggesting that QAMS was a reliable and convenient method for the content determination of multiple components.The HCA and OPLS-DA methods drew a similar conclusion.The 53 batches of SXNI samples from 7 manufacturers were categorized into five groups,indicating that chemometrics could reveal the quality differences of SXNI between the manufacturers.Conclusions:The method established herein was efficient and successful in assessing the quality of SXNI,and that it may be potentially employed in the quality control of related products composed of Ginkgo biloba extract.展开更多
In order to study the hydrolytic characterization of an anti-inflammatory prodrug （ RI-1 ） in vitro, an effective, accurate and reliable method for the simultaneous determination of the prodrug and its two hydrolyti...In order to study the hydrolytic characterization of an anti-inflammatory prodrug （ RI-1 ） in vitro, an effective, accurate and reliable method for the simultaneous determination of the prodrug and its two hydrolytic active compounds is developed using reverse phase high-performance liquid chromatography （RP-HPLC）. The chromatographic separation is performed on an ODS-2 C18 column （250 mm × 4. 6 mm, 5.0 μm particle size） with a simple elution program. The mobile phase is V（ methanol） ： V（0. 1% phosphoric acid solution） =90：10 （adjust pH to 2. 3）. A wavelength of 225 nm and a mobile phase flow rate of 1.0 mL/min are utilized for the quantitative analysis. Excellent linear behaviors over the investigated concentration ranges are observed with values of R2 higher than 0. 999 for all the analytes. The validated method is successfully applied to the simultaneous determination of the prodrug and its active components can be used to detect hydrolytic characterization in vitro.展开更多
A new institutional clinical trial assessed the improvement of sleep disorders in 40 children with autism treated by immediate-release melatonin formulation in different regimens(0.5 mg, 2 mg, and 6 mg daily) for one ...A new institutional clinical trial assessed the improvement of sleep disorders in 40 children with autism treated by immediate-release melatonin formulation in different regimens(0.5 mg, 2 mg, and 6 mg daily) for one month. The objectives of present study were to(i) prepare low-dose melatonin hard capsules for pediatric use controlled by two complementary methods and(ii) carry out a stability study in order to determine a use-bydate. Validation of preparation process was claimed as ascertained by mass uniformity of hard capsules.Multicomponent analysis by attenuated total reflectance Fourier transformed infrared(ATR-FTIR) of melatonin/microcrystalline cellulose mixture allowed to identify and quantify relative content of active pharmaceutical ingredients and excipients. Absolute melatonin content analysis by high performance liquid chromatography in 0.5 mg and 6 mg melatonin capsules was 93.6% ± 4.1% and 98.7% ± 6.9% of theoretical value, respectively. Forced degradation study showed a good separation of melatonin and its degradation products. The capability of the method was 15, confirming a risk of false negative < 0.01%. Stability test and dissolution test were compliant over 18 months of storage with European Pharmacopoeia. Preparation of melatonin hard capsules was completed manually and melatonin in hard capsules was stable for 18 months, in spite of low doses of active ingredient. ATR-FTIR offers a real alternative to HPLC for quality control of highdose melatonin hard capsules before the release of clinical batches.展开更多
目的建立扣子七的超高效液相(ultra high performance liquid chromatography,UPLC)指纹图谱,同时建立一测多评法(quantitative analysis of multi-components by single marker,QAMS)对8个化学成分进行含量测定,并结合化学模式识别分...目的建立扣子七的超高效液相(ultra high performance liquid chromatography,UPLC)指纹图谱,同时建立一测多评法(quantitative analysis of multi-components by single marker,QAMS)对8个化学成分进行含量测定,并结合化学模式识别分析对扣子七进行质量评价。方法采用Waters CORTECS UPLC T3色谱柱,以0.1%磷酸水-乙腈溶液为流动相进行梯度洗脱,柱温30℃,流速0.3 mL·min^(-1),建立扣子七UPLC指纹图谱,进行聚类分析、主成分分析和正交偏最小二乘法-判别分析,并以竹节参皂苷Ⅳa为内标,建立人参皂苷Rb1、人参皂苷Ro、人参皂苷Rb3、竹节参皂苷Ⅳ、人参皂苷Rd、姜状三七皂苷R1和金盏花苷E的相对校正因子,计算8种成分的含量,并与外标法测定结果进行比较,以验证QAMS方法的准确性、重复性及可行性。结果14批指纹图谱共确定12个共有峰,指认人参皂苷Rb1、人参皂苷Ro、人参皂苷Rb3、竹节参皂苷Ⅳ、竹节参皂苷Ⅳa、人参皂苷Rd、姜状三七皂苷R1和金盏花苷E 8种主要特征成分。14批样品图谱的相似度在0.793~0.993之间,聚类分析可将14批样品分为4类,主成分分析得到4个主成分,累计方差贡献率为83.20%,正交偏最小二乘法-判别分析筛选出5个差异质量标志物。QAMS法计算值与外标法实测值无统计学差异。结论该研究建立的扣子七UPLC指纹图谱结合一测多评法简便可行,结合化学模式识别可有效为扣子七药材整体质量控制提供参考。展开更多
[Objectives]The purpose of this study was to establish a method for the determination of five kinds of flavonoids in trichosanthes peel.[Methods]The contents of rutin,isoquercitrin,quercitrin,quercetin and kaempferol ...[Objectives]The purpose of this study was to establish a method for the determination of five kinds of flavonoids in trichosanthes peel.[Methods]The contents of rutin,isoquercitrin,quercitrin,quercetin and kaempferol in trichosanthes peel samples collected from different sites were determined by high-performance liquid chromatography.With each component as an index,principal component analysis and cluster analysis were performed.[Results]The contents of flavonoids in the trichosanthes peel samples from different sites were different.The cumulative variance contribution rate of isoquercitrin was 95.514%.The results of cluster analysis show that the quality of trichosanthes peel from Anhui was the best.[Conclusions]Taking isoquercitrin as a common factor to carry out content determination will help to better control the quality of trichosanthes peel.展开更多
A high performance liquid chromatography-ultraviolet(HPLC-UV)fingerprint method for the overall chemical analysis of edible mushrooms was established based on Auricularia heimuer for the first time,and then applied to...A high performance liquid chromatography-ultraviolet(HPLC-UV)fingerprint method for the overall chemical analysis of edible mushrooms was established based on Auricularia heimuer for the first time,and then applied to analyze 60 batches of A.heimuer,Auricularia cornea.Auricularia cornea*Yu Muer’and TremeUa fuciformis.A total of 9 characteristic peaks of A.heimuer.11 characteristic peaks of A.cornea,6 characteristic peaks of A.cornea‘Yu Muer’,and 9 characteristic peaks of I fuciformis were designated.Then,a combinatory analysis,including similarity evaluation,hierarchical cluster analysis and principal component analysis,revealed the chemical consistency and difference between samples from the same and different species.The HPLC fingerprint method established in this paper could be used to characterize the components of A.heimuer,A.cornea,A.cornea‘Yu Muer’,and T.fuciformis and discriminate the 4 edible mushrooms effectively in combination with pattern recognition analysis.展开更多
基金the National Natural Science Foundation of China(No.90709021)Knowledge Innovation Program of Chi-nese Academy of Sciences(No.KJCX2.YW.HO9)
文摘Some natural products, such as traditional Chinese medicines（TCMs）, contain compounds with anticancer activity and have attracted a great interest in recent years as alternative anticancer therapies. A quick and convenient assay for screening antimicrotubule compounds in which in vitro microdialysis/high-performance liquid chromatography （HPLC） is used to monitor the binding of the compounds extracted from TCM Taxus cuspidata Siebold ＆ Zucc（Taxus） to microtubules is reported. It was observed that the extract of Taxus contains at least five compounds which have affinity interaction with microtubules by biological fingerprinting analysis, and they were identified as the taxoids of taxol, baccatin III, 10-deacetylbaccatin Ⅲ（10-DAB）, cephalomannine and 7-epi-10-deacetyltaxol （7-epi-10-DAT） based on the comparison of their high-performance liquid chromatographic/mass spectrometric and UV spectra with those of the standard samples, both assembly-promoting and disassembly-inhibiting characteristics of those compounds were evaluated. It was observed that baccatin Ⅲ and 10-DAB bound to microtubules and the binding degrees were influenced by GTP. Competitive binding behavior of taxol with other four taxoids to microtubules was also investigated.
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.
基金supported by the National Key Research and Development Program of China(No.2018YFC1707904,2018YFC1707900)。
文摘Objective:Belamcandae Rhizoma and Iridis Tectori Rhizoma are easily confused with each other.The main objective of this study is to distinguish them using chemical analysis.Materials and Methods:Thin-layer chromatography(TLC)and high-performance liquid chromatography(HPLC)fingerprint methods were established to compare the chemical profile,while HPLC quantitation was used to determine the contents of three isoflavones in thirty batches of Belamcandae Rhizoma and Iridis Tectori Rhizoma samples.Results:The two herbs could be distinguished by TLC using acetic acid-n hexane-ethyl acetate(1:90:80 v/v/v)as the mobile phase,according to the fluorescent band under 366 nm at R_(f) 0.2.In total,12 compounds were identified in the 24-min HPLC fingerprint.The similarity coefficient between the two herbs was 0.54±0.01.Mangiferin(1),tectoridin(2),iridin(3),irigenin(5),irisflorentin(6),and iristectorin A(9)were the main peaks in Belamcandae Rhizoma,while tectoridin(2)and tectorigenin(4)were the major peaks in Iridis Tectori Rhizoma.The contents of 2 in Iridis Tectori Rhizoma(2.50±0.20%)were 8.93 times higher than that of Belamcandae Rhizoma(0.28±0.08%),while the ones of 5 and 6 were slightly lower in Iridis Tectori Rhizoma.Conclusions:The study established fast and effective methods to distinguish Belamcandae Rhizoma from Iridis Tectori Rhizoma.
基金supported financially by the Guangxi Science and Technology Research Project(GuiKeAA18242040)the National Science and Technology Major Project(2018ZX09735-002)。
文摘Objective:In this study,a comprehensive and effective quality method for evaluating the efficacy of ShuXueNing injection(SXNI)was developed.Materials and Methods:Quantitative high-performance liquid chromatography fingerprint,the quantitative analysis of multicomponents by a single marker(QAMS)method,hierarchical cluster analysis(HCA),and orthogonal partial least squares discrimination analysis(OPLS-DA)were used to distinguish 53 batches of SXNI samples from 7 manufacturers.Results:A total of 53 batches of samples were analyzed to establish antithesis fingerprint of SXNI,and 12 peaks of the common model were collected and used for the similarity analysis.Meanwhile,six index flavonoid components were determined by the QAMS method,using rutin as internal reference substance.The accuracy of the QAMS method was confirmed by investigating the relative deviation between the QAMS method and the traditional external standard method.The results demonstrated that there was no significant difference(RE<1%),suggesting that QAMS was a reliable and convenient method for the content determination of multiple components.The HCA and OPLS-DA methods drew a similar conclusion.The 53 batches of SXNI samples from 7 manufacturers were categorized into five groups,indicating that chemometrics could reveal the quality differences of SXNI between the manufacturers.Conclusions:The method established herein was efficient and successful in assessing the quality of SXNI,and that it may be potentially employed in the quality control of related products composed of Ginkgo biloba extract.
文摘In order to study the hydrolytic characterization of an anti-inflammatory prodrug （ RI-1 ） in vitro, an effective, accurate and reliable method for the simultaneous determination of the prodrug and its two hydrolytic active compounds is developed using reverse phase high-performance liquid chromatography （RP-HPLC）. The chromatographic separation is performed on an ODS-2 C18 column （250 mm × 4. 6 mm, 5.0 μm particle size） with a simple elution program. The mobile phase is V（ methanol） ： V（0. 1% phosphoric acid solution） =90：10 （adjust pH to 2. 3）. A wavelength of 225 nm and a mobile phase flow rate of 1.0 mL/min are utilized for the quantitative analysis. Excellent linear behaviors over the investigated concentration ranges are observed with values of R2 higher than 0. 999 for all the analytes. The validated method is successfully applied to the simultaneous determination of the prodrug and its active components can be used to detect hydrolytic characterization in vitro.
文摘A new institutional clinical trial assessed the improvement of sleep disorders in 40 children with autism treated by immediate-release melatonin formulation in different regimens(0.5 mg, 2 mg, and 6 mg daily) for one month. The objectives of present study were to(i) prepare low-dose melatonin hard capsules for pediatric use controlled by two complementary methods and(ii) carry out a stability study in order to determine a use-bydate. Validation of preparation process was claimed as ascertained by mass uniformity of hard capsules.Multicomponent analysis by attenuated total reflectance Fourier transformed infrared(ATR-FTIR) of melatonin/microcrystalline cellulose mixture allowed to identify and quantify relative content of active pharmaceutical ingredients and excipients. Absolute melatonin content analysis by high performance liquid chromatography in 0.5 mg and 6 mg melatonin capsules was 93.6% ± 4.1% and 98.7% ± 6.9% of theoretical value, respectively. Forced degradation study showed a good separation of melatonin and its degradation products. The capability of the method was 15, confirming a risk of false negative < 0.01%. Stability test and dissolution test were compliant over 18 months of storage with European Pharmacopoeia. Preparation of melatonin hard capsules was completed manually and melatonin in hard capsules was stable for 18 months, in spite of low doses of active ingredient. ATR-FTIR offers a real alternative to HPLC for quality control of highdose melatonin hard capsules before the release of clinical batches.
文摘目的建立扣子七的超高效液相(ultra high performance liquid chromatography,UPLC)指纹图谱,同时建立一测多评法(quantitative analysis of multi-components by single marker,QAMS)对8个化学成分进行含量测定,并结合化学模式识别分析对扣子七进行质量评价。方法采用Waters CORTECS UPLC T3色谱柱,以0.1%磷酸水-乙腈溶液为流动相进行梯度洗脱,柱温30℃,流速0.3 mL·min^(-1),建立扣子七UPLC指纹图谱,进行聚类分析、主成分分析和正交偏最小二乘法-判别分析,并以竹节参皂苷Ⅳa为内标,建立人参皂苷Rb1、人参皂苷Ro、人参皂苷Rb3、竹节参皂苷Ⅳ、人参皂苷Rd、姜状三七皂苷R1和金盏花苷E的相对校正因子,计算8种成分的含量,并与外标法测定结果进行比较,以验证QAMS方法的准确性、重复性及可行性。结果14批指纹图谱共确定12个共有峰,指认人参皂苷Rb1、人参皂苷Ro、人参皂苷Rb3、竹节参皂苷Ⅳ、竹节参皂苷Ⅳa、人参皂苷Rd、姜状三七皂苷R1和金盏花苷E 8种主要特征成分。14批样品图谱的相似度在0.793~0.993之间,聚类分析可将14批样品分为4类,主成分分析得到4个主成分,累计方差贡献率为83.20%,正交偏最小二乘法-判别分析筛选出5个差异质量标志物。QAMS法计算值与外标法实测值无统计学差异。结论该研究建立的扣子七UPLC指纹图谱结合一测多评法简便可行,结合化学模式识别可有效为扣子七药材整体质量控制提供参考。
基金College Students'Innovation and Entrepreneurship Training Program of Liaoning Province(201911430039).
文摘[Objectives]The purpose of this study was to establish a method for the determination of five kinds of flavonoids in trichosanthes peel.[Methods]The contents of rutin,isoquercitrin,quercitrin,quercetin and kaempferol in trichosanthes peel samples collected from different sites were determined by high-performance liquid chromatography.With each component as an index,principal component analysis and cluster analysis were performed.[Results]The contents of flavonoids in the trichosanthes peel samples from different sites were different.The cumulative variance contribution rate of isoquercitrin was 95.514%.The results of cluster analysis show that the quality of trichosanthes peel from Anhui was the best.[Conclusions]Taking isoquercitrin as a common factor to carry out content determination will help to better control the quality of trichosanthes peel.
基金This publication was financially supported by the National Key R&D Program of China(2018YFD0400202 and 2018YFD0400200).
文摘A high performance liquid chromatography-ultraviolet(HPLC-UV)fingerprint method for the overall chemical analysis of edible mushrooms was established based on Auricularia heimuer for the first time,and then applied to analyze 60 batches of A.heimuer,Auricularia cornea.Auricularia cornea*Yu Muer’and TremeUa fuciformis.A total of 9 characteristic peaks of A.heimuer.11 characteristic peaks of A.cornea,6 characteristic peaks of A.cornea‘Yu Muer’,and 9 characteristic peaks of I fuciformis were designated.Then,a combinatory analysis,including similarity evaluation,hierarchical cluster analysis and principal component analysis,revealed the chemical consistency and difference between samples from the same and different species.The HPLC fingerprint method established in this paper could be used to characterize the components of A.heimuer,A.cornea,A.cornea‘Yu Muer’,and T.fuciformis and discriminate the 4 edible mushrooms effectively in combination with pattern recognition analysis.
