A combined method of high performance liquid chromatograph-elecrtrospray-ionization mass spectrometer（HPLC-ESI-MS/MS） coupled with a photodiode array detector（HPLC-DAD） and principal component analysis（PCA） was ...A combined method of high performance liquid chromatograph-elecrtrospray-ionization mass spectrometer（HPLC-ESI-MS/MS） coupled with a photodiode array detector（HPLC-DAD） and principal component analysis（PCA） was applied to the qualitative and quantitative analyses of alkaloids in Cortex Phellodendri（CP） samples, and to the differentiation of two species of CP, Cortex Phellodendri Chinensis（CPC） and Cortex Phellodendri Amurensis（CPA）. Twenty-two peaks appeared in the HPLC-MS base peak chromatogram of CP detected by the HPLC-ESI-MS/MS analysis, and the alkaloids were identified according to the MSn data, the known MS fragmentation rules and the literature data. Five alkaloids including berberine, palmatine, jatrorrhizine, phellodendrine and magnoflorine were simultaneously determinated by the HPLC-DAD. Berberine was the primary component in all CP samples, and the contents of berberine and palmatine were exploited to be two critical parameters for effective discrimination between the two species of CP. The average content of berberine in CPC（58.75 mg/g） was higher than that in CPA（9.16 mg/g）, while the content of palmatine was less, only 0.25 mg/g in CPC and 4.19 mg/g in CPA. With the use of PCA, samples datasets were separated successfully into two different clusters corresponding to the two species, and berberine, pahnatine, phellodendrine and magnoflorine contribute most to the above mentioned calssifying . The proposed method oroved to be a useful tool in the aualitv control of Chinese herbal medicines.展开更多
[Objectives]To establish a multi-indicator quality control method for the retention of Longqing Capsule based on the principle of prescription of Chinese medicine.[Methods]High performance liquid chromatography(HPLC)w...[Objectives]To establish a multi-indicator quality control method for the retention of Longqing Capsule based on the principle of prescription of Chinese medicine.[Methods]High performance liquid chromatography(HPLC)with ShimNex CS C 18 as the column;column temperature:35℃;wavelength:270 nm;methanol-0.1%phosphoric acid solution as the mobile phase with gradient elution.[Results]The 12 components of the retention of Longqing Capsule showed good linearity within the investigated range(r≥0.9995),with the average spiked recoveries of 97.83%-100.52%and the RSD of 0.9%-2.1%.[Conclusions]The method is exclusive,sensitive,reproducible,simple and easy to use,and can provide a reference for the construction of the quality standard and control system of Longqing Capsule based on the theory of traditional Chinese medicine.展开更多
A new set of descriptors, HSEHPCSV （component score vector of hydrophobic, steric, and electronic properties together with hydrogen bonding contributions）, were derived from principal component analyses of 95 physic...A new set of descriptors, HSEHPCSV （component score vector of hydrophobic, steric, and electronic properties together with hydrogen bonding contributions）, were derived from principal component analyses of 95 physicochemical variables of 20 natural amino acids separately according to different kinds of properties described, namely, hydrophobic, steric, and electronic properties as well as hydrogen bonding contributions. HSEHPCSV scales were then employed to express structures of angiotensin-converting enzyme inhibitors, bitter tasting thresholds and bactericidal 18 peptide, and to construct QSAR models based on partial least square （PLS）. The results obtained are as follows： the multiple correlation coefficient （R2cum） of 0.846, 0.917 and 0.993, leave-one-out cross validated Q2cm of 0.835, 0.865 and 0.899, and root-mean-square error for estimated error （RMSEE） of 0.396, 0.187and 0.22, respectively. Satisfactory results showed that, as new amino acid scales, data of HSEHPCSV may be a useful structural expression methodology＇for the studies on peptide QSAR （quantitative structure-activity relationship） due to many advantages such as plentiful structural information, definite physical and chemical meaning and easy interpretation.展开更多
Software projects influenced by many human factors generate various risks. In order to develop highly quality software, it is important to respond to these risks reasonably and promptly. In addition, it is not easy fo...Software projects influenced by many human factors generate various risks. In order to develop highly quality software, it is important to respond to these risks reasonably and promptly. In addition, it is not easy for project managers to deal with these risks completely. Therefore, it is essential to manage the process quality by promoting activities of process monitoring and design quality assessment. In this paper, we discuss statistical data analysis for actual project management activities in process monitoring and design quality assessment, and analyze the effects for these software process improvement quantitatively by applying the methods of multivariate analysis. Then, we show how process factors affect the management measures of QCD (Quality, Cost, Delivery) by applying the multiple regression analyses to observed process monitoring data. Further, we quantitatively evaluate the effect by performing design quality assessment based on the principal component analysis and the factor analysis. As a result of analysis, we show that the design quality assessment activities are so effective for software process improvement. Further, based on the result of quantitative project assessment, we discuss the usefulness of process monitoring progress assessment by using a software reliability growth model. This result may enable us to give a useful quantitative measure of product release determination.展开更多
In modern processing of conducting materials, such as steel,the time-varying electromagnetic field plays a key role in obtaining the desired microstructure or eliminating solidification defects such as porosity and se...In modern processing of conducting materials, such as steel,the time-varying electromagnetic field plays a key role in obtaining the desired microstructure or eliminating solidification defects such as porosity and segregation in cast billets. Up to now,few studies on the induced electromagnetic force （also called the Lorentz force） field in liquid metal have been reported. Compared with the magnetic field, the induced force field is the real and only direct cause for flow control. The electromagnetic force is comprised of two components. One is time-independent and the other is time- dependent. The time-dependent component varies with time in both amplitude and direction. When it reaches the extreme value,it can be one dozen times larger than the time-independent component. In this paper, a new method to quantitatively describe the induced electromagnetic force in liquid metal under a harmonic electromagnetic field,including both its time- independent and dependent components, was proposed based on the formula derivation from the data of amplitude and phase angle. Through this method ,the features of the time-dependent component were discussed, including the directions of rotation and the long axis. As a result, the force pattern was described. With two example calculations, the method was explained in detail. The results of both examples show that the force field in liquid metal can be divided into several regions with different force features. Example 1 shows the effect of coil position on the evolution of the force field pattern in liquid metal. Example 2 is a kind of stirring by the travelling magnetic field ,whose results present the sub-structures in metal and show that most of them have almost the same rotating direction.展开更多
[Objectives]To regulate the quality of Wanjinxiang Shushuang Ointment through simultaneously quantifying menthol,camphor,1,8-cineole,linalool,borneol and caryophyllene oxide by QAMS(quantitative analysis of multi-comp...[Objectives]To regulate the quality of Wanjinxiang Shushuang Ointment through simultaneously quantifying menthol,camphor,1,8-cineole,linalool,borneol and caryophyllene oxide by QAMS(quantitative analysis of multi-components by single-marker).[Methods]The method was performed using an Agilent DB-WAX(30 m×0.32 mm,0.25μm)polyethylene glycol chromatographic column;with nitrogen employed as a carrier gas.The constant pressure was 4.73 psi;and the injection temperature was 240℃,with a shunt ratio:of 10:1;The hydrogen flame ion detector with a detector temperature of 240℃;the injection volume was 0.3μL.To verify the accuracy and applicability of QAMS,the results were compared with those obtained using the internal standard method(naphthalene).[Results]In Wanjinxiang Shushuang Ointment,menthol,camphor,1,8-cineole,linalool,borneol,caryophyllene oxide and naphthalene were well separated by the same chromatography with good linearity in their respective ranges(R≥0.9992).The average recoveries were 99.66%,101.03%,98.07%,98.24%,101.39%,and 103.39%with RSD s of 0.69%,1.52%,1.25%,1.94%,1.44%,and 2.74%,respectively.The QAMS is similar to the internal standard method.[Conclusions]This simple,accurate method with high precision,separation and reproducibility can serve as a reference for the quality control of Wanjinxiang Shushuang Ointment.展开更多
目的建立美洲大蠊的HPLC指纹图谱,并运用一测多评法(quantitative analysis of multi-components with a singlemarker,QAMS)测定9种氨基酸的含量,综合评价美洲大蠊氨基酸质量差异。方法样品在6 mol∙L^(−1)盐酸溶液中120℃水解6 h,再与...目的建立美洲大蠊的HPLC指纹图谱,并运用一测多评法(quantitative analysis of multi-components with a singlemarker,QAMS)测定9种氨基酸的含量,综合评价美洲大蠊氨基酸质量差异。方法样品在6 mol∙L^(−1)盐酸溶液中120℃水解6 h,再与异硫氰酸苯酯(phenylisothiocyanate,PITC)40℃水浴1 h进行衍生化反应。衍生化产物分析采用Kromasil 100-5-C_(18)色谱柱(4.6 mm×250 mm,5μm),以0.1 mol∙L^(−1)乙酸钠溶液(pH 6.5±0.05)-乙腈(97∶3)为流动相A,乙腈-水(4∶1)为流动相B,梯度洗脱,流速0.8 mL∙min^(−1),检测波长254 nm,柱温40℃,进样量2μL。对指纹图谱进行相似度评价、聚类分析(cluster analysis,CA)、主成分分析(principal component analysis,PCA)、正交偏最小二乘法-判别分析(orthogonal partial least squares discriminant analysis,OPLS-DA)。建立内参物丙氨酸与甘氨酸、精氨酸、苏氨酸、酪氨酸、缬氨酸、异亮氨酸、亮氨酸及苯丙氨酸的相对校正因子(f)并对其耐用性考察。采用外标法(external standard method,ESM)与QAMS分别测定16批美洲大蠊中9个氨基酸含量,并用独立样本t检验比较验证QAMS方法的准确性。结果采用中药色谱指纹图谱相似度评价系统(2004A版)、SPSS 27.0与SIMCA 14.1分析16批美洲大蠊的氨基酸指纹图谱:标定17个共有峰,明确15个已知成分;16批次的相似度在0.888~0.982,表明其质量一致性较好;CA与PCA结果均分为3大类,意味着不同产地质量存在一定差异;OPLS-DA筛选了脯氨酸、赖氨酸、缬氨酸、异亮氨酸、苏氨酸、亮氨酸、丙氨酸及共有峰9共8个主要的质量差异标志物。含量测定方面,9个成分的专属性、线性关系(r≥0.9999)、精密度、重复性、稳定性均良好,平均加样回收率在98.70%~101.93%,RSD在1.05%~2.24%。QAMS方法学验证内参物丙氨酸与8个氨基酸的f分别为甘氨酸0.8338、精氨酸1.9641、苏氨酸1.4489、酪氨酸1.8306、缬氨酸1.2767、异亮氨酸1.3816、亮氨酸1.4082、苯丙氨酸1.6542。t检验结果ESM法与QAMS法含量测定结果差异无统计学意义。结论本研究所构建的HPLC指纹图谱与QAMS结合方法操作简便、专属性强、重现性好,能够有效评价美洲大蠊氨基酸的组成,为美洲大蠊药材及其提取物中氨基酸成分的质量控制奠定理论基础。展开更多
目的比较功能定量磁化率成像(fQSM)和血氧水平依赖(BOLD)成像在对指任务功能MRI(fMRI)中检测脑激活的能力。方法前瞻性招募24例健康成人志愿者,采用3.0 T MRI设备同步采集对指运动任务的fMRI幅度及相位图。采用一般线性模型(GLM)和独立...目的比较功能定量磁化率成像(fQSM)和血氧水平依赖(BOLD)成像在对指任务功能MRI(fMRI)中检测脑激活的能力。方法前瞻性招募24例健康成人志愿者,采用3.0 T MRI设备同步采集对指运动任务的fMRI幅度及相位图。采用一般线性模型(GLM)和独立成分分析(ICA)成像提取任务诱发的BOLD以及fQSM脑激活图。采用相关分析探讨BOLD和f QSM脑激活成分时间序列的相似性,采用配对t检验或置换检验比较BOLD和fQSM脑激活成分动态范围和分数低频振幅的差别。结果GLM显示BOLD激活脑区主要位于双侧中央前后回和小脑运动区,而fQSM未检测到激活的脑区(体素水平P<0.001,团块水平FWEc校正P<0.05)。即使降低阈值,fQSM检测到的激活也远少于BOLD,且两者在小脑运动区的时间序列呈显著负相关。头动和空间平滑对BOLD及fQSM激活强度的影响不显著。固定成分数(90)的ICA显示,BOLD能敏感检测到与对指任务时序密切关联的脑激活独立成分,而fQSM未能检测到与任务相关的脑激活,BOLD和fQSM各激活成分时间序列相关性较弱,且BOLD激活成分时间序列的动态范围和分数低频振幅显著高于fQSM(P<0.05,Bonferroni校正)。此外,自动成分数选择的ICA识别到3个与运动显著关联的f QSM脑激活成分,包括感觉运动、内侧前额叶和小脑运动网络,且后者与BOLD感觉运动网络存在显著负相关。结论fQSM技术在手指运动相关脑激活方面的检测能力低于BOLD技术,使用自动成分数选择的ICA有助于提高fQSM脑激活检测能力。展开更多
目的建立积雪草提取物的薄层色谱法(thin-layer chromatography,TLC)鉴别方法和高效液相色谱定量方法,并结合一测多评法(quantitative analysis of multi-components by single marker,QAMS)实现积雪草苷、积雪草苷B和羟基积雪草苷的定...目的建立积雪草提取物的薄层色谱法(thin-layer chromatography,TLC)鉴别方法和高效液相色谱定量方法,并结合一测多评法(quantitative analysis of multi-components by single marker,QAMS)实现积雪草苷、积雪草苷B和羟基积雪草苷的定量测定。方法首先采用TLC对积雪草提取物进行定性鉴别,确保样品的真实性;其次采用高效液相色谱法进行含量测定,流动相分别为2 mmol/Lβ-环糊精溶液和乙腈,检测波长为205 nm。以羟基积雪草苷为参照物,计算其他两种物质的相对校正因子,并将测定含量与外标法测定结果进行比较。结果3种成分在10~500 mg/L范围内线性关系良好,不同浓度水平的加标回收率范围为87.0%~108.2%,相对标准偏差为3.1%~5.2%,方法具有良好的精密度、重复性和稳定性。QAMS与外标法测定积雪草提取物中3种特征性成分的含量一致性良好。结论TLC鉴别方法结合QAMS方法实现定性定量检测,能够对积雪草提取物的质量控制提供技术支持。展开更多
目的建立一测多评法(quantitative analysis of multi-components by single marker,QAMS)同时测定小陷胸汤中次黄嘌呤、香草酸、木兰花碱、去亚甲基小檗碱、非洲防己碱、药根碱、盐酸黄连碱、盐酸巴马汀、盐酸小檗碱的含量。方法本实...目的建立一测多评法(quantitative analysis of multi-components by single marker,QAMS)同时测定小陷胸汤中次黄嘌呤、香草酸、木兰花碱、去亚甲基小檗碱、非洲防己碱、药根碱、盐酸黄连碱、盐酸巴马汀、盐酸小檗碱的含量。方法本实验采用色谱柱Spursil C18(4.6 mm×250 mm,5μm),以乙腈-0.05 mol·L-1磷酸二氢钾溶液加磷酸调pH=4.0为流动相,检测波长:0~20 min:290 nm;20~45 min:300 nm,柱温30℃,进样量10μL。以盐酸小檗碱为内参物,分别计算其余8个成分的相对校正因子并计算各成分含量,比较外标法(external standard method,ESM)和QAMS法结果的差异。结果小陷胸汤9个成分在一定浓度范围与峰面积呈良好的线性关系(r>0.9980),平均加样回收率为94.36%~105.57%,相对标准偏差(relative standard deviation,RSD)为0.52%~3.48%,QAMS法与ESM法测定的结果无显著性差异。结论本研究建立的小陷胸汤QAMS法结果准确可靠,该方法简便易行,可用于小陷胸汤的质量控制。展开更多
基金Supported by the National Natural Science Foundation of China(No30725045)the Foundation of Eleventh Five-Year-Plan of China(No2008ZX09202-002)+1 种基金the Shanghai Leading Academic Discipline Project, China(NoB906)the Scientific Foundation of Shanghai City, China(No07DZ19702)
文摘A combined method of high performance liquid chromatograph-elecrtrospray-ionization mass spectrometer（HPLC-ESI-MS/MS） coupled with a photodiode array detector（HPLC-DAD） and principal component analysis（PCA） was applied to the qualitative and quantitative analyses of alkaloids in Cortex Phellodendri（CP） samples, and to the differentiation of two species of CP, Cortex Phellodendri Chinensis（CPC） and Cortex Phellodendri Amurensis（CPA）. Twenty-two peaks appeared in the HPLC-MS base peak chromatogram of CP detected by the HPLC-ESI-MS/MS analysis, and the alkaloids were identified according to the MSn data, the known MS fragmentation rules and the literature data. Five alkaloids including berberine, palmatine, jatrorrhizine, phellodendrine and magnoflorine were simultaneously determinated by the HPLC-DAD. Berberine was the primary component in all CP samples, and the contents of berberine and palmatine were exploited to be two critical parameters for effective discrimination between the two species of CP. The average content of berberine in CPC（58.75 mg/g） was higher than that in CPA（9.16 mg/g）, while the content of palmatine was less, only 0.25 mg/g in CPC and 4.19 mg/g in CPA. With the use of PCA, samples datasets were separated successfully into two different clusters corresponding to the two species, and berberine, pahnatine, phellodendrine and magnoflorine contribute most to the above mentioned calssifying . The proposed method oroved to be a useful tool in the aualitv control of Chinese herbal medicines.
基金Supported by Provincial University Scientific Research Platform Team Project of Guizhou Provincial Department of Education(Qianjiaoji[2022]No.010).
文摘[Objectives]To establish a multi-indicator quality control method for the retention of Longqing Capsule based on the principle of prescription of Chinese medicine.[Methods]High performance liquid chromatography(HPLC)with ShimNex CS C 18 as the column;column temperature:35℃;wavelength:270 nm;methanol-0.1%phosphoric acid solution as the mobile phase with gradient elution.[Results]The 12 components of the retention of Longqing Capsule showed good linearity within the investigated range(r≥0.9995),with the average spiked recoveries of 97.83%-100.52%and the RSD of 0.9%-2.1%.[Conclusions]The method is exclusive,sensitive,reproducible,simple and easy to use,and can provide a reference for the construction of the quality standard and control system of Longqing Capsule based on the theory of traditional Chinese medicine.
基金Supported by the National High Technology Research and Development Program of China (863 Program, No. 2006AA02Z312)
文摘A new set of descriptors, HSEHPCSV （component score vector of hydrophobic, steric, and electronic properties together with hydrogen bonding contributions）, were derived from principal component analyses of 95 physicochemical variables of 20 natural amino acids separately according to different kinds of properties described, namely, hydrophobic, steric, and electronic properties as well as hydrogen bonding contributions. HSEHPCSV scales were then employed to express structures of angiotensin-converting enzyme inhibitors, bitter tasting thresholds and bactericidal 18 peptide, and to construct QSAR models based on partial least square （PLS）. The results obtained are as follows： the multiple correlation coefficient （R2cum） of 0.846, 0.917 and 0.993, leave-one-out cross validated Q2cm of 0.835, 0.865 and 0.899, and root-mean-square error for estimated error （RMSEE） of 0.396, 0.187and 0.22, respectively. Satisfactory results showed that, as new amino acid scales, data of HSEHPCSV may be a useful structural expression methodology＇for the studies on peptide QSAR （quantitative structure-activity relationship） due to many advantages such as plentiful structural information, definite physical and chemical meaning and easy interpretation.
文摘Software projects influenced by many human factors generate various risks. In order to develop highly quality software, it is important to respond to these risks reasonably and promptly. In addition, it is not easy for project managers to deal with these risks completely. Therefore, it is essential to manage the process quality by promoting activities of process monitoring and design quality assessment. In this paper, we discuss statistical data analysis for actual project management activities in process monitoring and design quality assessment, and analyze the effects for these software process improvement quantitatively by applying the methods of multivariate analysis. Then, we show how process factors affect the management measures of QCD (Quality, Cost, Delivery) by applying the multiple regression analyses to observed process monitoring data. Further, we quantitatively evaluate the effect by performing design quality assessment based on the principal component analysis and the factor analysis. As a result of analysis, we show that the design quality assessment activities are so effective for software process improvement. Further, based on the result of quantitative project assessment, we discuss the usefulness of process monitoring progress assessment by using a software reliability growth model. This result may enable us to give a useful quantitative measure of product release determination.
文摘In modern processing of conducting materials, such as steel,the time-varying electromagnetic field plays a key role in obtaining the desired microstructure or eliminating solidification defects such as porosity and segregation in cast billets. Up to now,few studies on the induced electromagnetic force （also called the Lorentz force） field in liquid metal have been reported. Compared with the magnetic field, the induced force field is the real and only direct cause for flow control. The electromagnetic force is comprised of two components. One is time-independent and the other is time- dependent. The time-dependent component varies with time in both amplitude and direction. When it reaches the extreme value,it can be one dozen times larger than the time-independent component. In this paper, a new method to quantitatively describe the induced electromagnetic force in liquid metal under a harmonic electromagnetic field,including both its time- independent and dependent components, was proposed based on the formula derivation from the data of amplitude and phase angle. Through this method ,the features of the time-dependent component were discussed, including the directions of rotation and the long axis. As a result, the force pattern was described. With two example calculations, the method was explained in detail. The results of both examples show that the force field in liquid metal can be divided into several regions with different force features. Example 1 shows the effect of coil position on the evolution of the force field pattern in liquid metal. Example 2 is a kind of stirring by the travelling magnetic field ,whose results present the sub-structures in metal and show that most of them have almost the same rotating direction.
基金Supported by Projects of Guizhou Provincial Department of Education-Growth Program of Young Scientific and Technological Talents in Guizhou Ordinary Higher Education Institutions(QJHKY[2022]264)Rolling Support for Provincial University Research Platform Team Projects(QJJ[2022]010).
文摘[Objectives]To regulate the quality of Wanjinxiang Shushuang Ointment through simultaneously quantifying menthol,camphor,1,8-cineole,linalool,borneol and caryophyllene oxide by QAMS(quantitative analysis of multi-components by single-marker).[Methods]The method was performed using an Agilent DB-WAX(30 m×0.32 mm,0.25μm)polyethylene glycol chromatographic column;with nitrogen employed as a carrier gas.The constant pressure was 4.73 psi;and the injection temperature was 240℃,with a shunt ratio:of 10:1;The hydrogen flame ion detector with a detector temperature of 240℃;the injection volume was 0.3μL.To verify the accuracy and applicability of QAMS,the results were compared with those obtained using the internal standard method(naphthalene).[Results]In Wanjinxiang Shushuang Ointment,menthol,camphor,1,8-cineole,linalool,borneol,caryophyllene oxide and naphthalene were well separated by the same chromatography with good linearity in their respective ranges(R≥0.9992).The average recoveries were 99.66%,101.03%,98.07%,98.24%,101.39%,and 103.39%with RSD s of 0.69%,1.52%,1.25%,1.94%,1.44%,and 2.74%,respectively.The QAMS is similar to the internal standard method.[Conclusions]This simple,accurate method with high precision,separation and reproducibility can serve as a reference for the quality control of Wanjinxiang Shushuang Ointment.
文摘目的比较功能定量磁化率成像(fQSM)和血氧水平依赖(BOLD)成像在对指任务功能MRI(fMRI)中检测脑激活的能力。方法前瞻性招募24例健康成人志愿者,采用3.0 T MRI设备同步采集对指运动任务的fMRI幅度及相位图。采用一般线性模型(GLM)和独立成分分析(ICA)成像提取任务诱发的BOLD以及fQSM脑激活图。采用相关分析探讨BOLD和f QSM脑激活成分时间序列的相似性,采用配对t检验或置换检验比较BOLD和fQSM脑激活成分动态范围和分数低频振幅的差别。结果GLM显示BOLD激活脑区主要位于双侧中央前后回和小脑运动区,而fQSM未检测到激活的脑区(体素水平P<0.001,团块水平FWEc校正P<0.05)。即使降低阈值,fQSM检测到的激活也远少于BOLD,且两者在小脑运动区的时间序列呈显著负相关。头动和空间平滑对BOLD及fQSM激活强度的影响不显著。固定成分数(90)的ICA显示,BOLD能敏感检测到与对指任务时序密切关联的脑激活独立成分,而fQSM未能检测到与任务相关的脑激活,BOLD和fQSM各激活成分时间序列相关性较弱,且BOLD激活成分时间序列的动态范围和分数低频振幅显著高于fQSM(P<0.05,Bonferroni校正)。此外,自动成分数选择的ICA识别到3个与运动显著关联的f QSM脑激活成分,包括感觉运动、内侧前额叶和小脑运动网络,且后者与BOLD感觉运动网络存在显著负相关。结论fQSM技术在手指运动相关脑激活方面的检测能力低于BOLD技术,使用自动成分数选择的ICA有助于提高fQSM脑激活检测能力。
文摘目的建立积雪草提取物的薄层色谱法(thin-layer chromatography,TLC)鉴别方法和高效液相色谱定量方法,并结合一测多评法(quantitative analysis of multi-components by single marker,QAMS)实现积雪草苷、积雪草苷B和羟基积雪草苷的定量测定。方法首先采用TLC对积雪草提取物进行定性鉴别,确保样品的真实性;其次采用高效液相色谱法进行含量测定,流动相分别为2 mmol/Lβ-环糊精溶液和乙腈,检测波长为205 nm。以羟基积雪草苷为参照物,计算其他两种物质的相对校正因子,并将测定含量与外标法测定结果进行比较。结果3种成分在10~500 mg/L范围内线性关系良好,不同浓度水平的加标回收率范围为87.0%~108.2%,相对标准偏差为3.1%~5.2%,方法具有良好的精密度、重复性和稳定性。QAMS与外标法测定积雪草提取物中3种特征性成分的含量一致性良好。结论TLC鉴别方法结合QAMS方法实现定性定量检测,能够对积雪草提取物的质量控制提供技术支持。
文摘目的建立一测多评法(quantitative analysis of multi-components by single marker,QAMS)同时测定小陷胸汤中次黄嘌呤、香草酸、木兰花碱、去亚甲基小檗碱、非洲防己碱、药根碱、盐酸黄连碱、盐酸巴马汀、盐酸小檗碱的含量。方法本实验采用色谱柱Spursil C18(4.6 mm×250 mm,5μm),以乙腈-0.05 mol·L-1磷酸二氢钾溶液加磷酸调pH=4.0为流动相,检测波长:0~20 min:290 nm;20~45 min:300 nm,柱温30℃,进样量10μL。以盐酸小檗碱为内参物,分别计算其余8个成分的相对校正因子并计算各成分含量,比较外标法(external standard method,ESM)和QAMS法结果的差异。结果小陷胸汤9个成分在一定浓度范围与峰面积呈良好的线性关系(r>0.9980),平均加样回收率为94.36%~105.57%,相对标准偏差(relative standard deviation,RSD)为0.52%~3.48%,QAMS法与ESM法测定的结果无显著性差异。结论本研究建立的小陷胸汤QAMS法结果准确可靠,该方法简便易行,可用于小陷胸汤的质量控制。
