Objective:To study the volatile constituents in different parts of Angelica sinensis for scientific evidence of its processing and clinical application.Methods:The volatile constituents in main and fibrous roots of Angelica sinensis were extracted by water distillation method and detected by GC-MS.The volatile constituents in main root were identified and determined by sub-window factor analysis (SFA) method.Then the volatile constituents in fibrous root were identified by orthogonal projection resolution (OPR).Results:67 and 65 components were identified in main root and fibrous root,respectively.They accounted for 89.68% and 87.07% of the total essential oil in main root and fibrous root,respectively.59 common components were identified in both main and fibrous roots including ligustilide,butylicene phthalide,2,6,6-trimethylbicyclo-[3,1,1] hept-2-ene,carvacrol,allo ocimene and 2-methoxy-4-vinylphenol.But the content of each component in main and fibrous roots varied.Conclusions:The proposed method could identify more components with improved accuracy,thus could be applied to analysis and quality control of traditional Chinese medicine from different plant parts or different habitants.
A method for the determination of finasteride in human plasma was developed by liquid chromatography-mass spectrometry.After deproteinization with acetonitrile,centrifugation,evaporation to dryness and dissolving in mobile phase,satisfactory separation was achieved on a Hypersil-Keystone C18 reversed-phase column using a mobile phase of acetonitrile-water(consisting 0.2% trifluoracetic)=55∶45(V/V).Carbamazepine(IS) was used as on internal standard.This method involved the use of the [M+H]+ ions of finasteride and IS at m/z373 and m/z237 with an electrospray ionization interface and the selective ion monitoring(SIM) mode.The calibration curve was linear in the range of 0.5-120 ng· mL-1(r=0.999).The limit of detection for finasteride in plasma was 0.02 ng· mL 1 (S/N=3).The inter-assay and intra-assay precision were in the range of 6.4 %-2.2 % and 5.5 %-1.7 %,respectively.The mean recoveries for spiking of 0.5 ng·mL-1,40 ng·mL-1 and 80 ng·mL 1 of finasteride in plasma were 108.5%,101.2% and 98.7%(n=6),respectively.The fast,accurate and sensitive method has been successfully used to estimate the pharmacokinetics of finasteride after its oral administration.
A simple, reliable and rapid isocratic liquid chromatography (LC)-mass spectrometric detection (MS) coupled with electrospray ionization (ESI) method for simultaneous separation and determination of calycosin-7-O-β-D-glucoside, ononin, calycosin and formonometin in Astragali Radix was developed. After the samples were extracted with ethanol, the optimum separation conditions for these analytes were achieved using water and acetonitrile (70:30, v/v) containing 0.2% (v/v) acetic acid as a mobile phase and a 2.0 mm×150 mm Hypersil-Keystone C18 column. Selective ion monitoring (SIM) mode and [M+H]+ ions at m/z 447, 431, 285 and 269 were used for quantitative analysis of four main active components above mentioned. The calibration curves were linear in the range of 0.4−175.0 μg/mL for calycosin-7-O-β-D-glucoside, 0.2−146.0 μg/mL for ononin, 0.4−210.0 μg/mL for calycosin and 0.5−217.0 μg/mL for formonetion, respectively. The limits of quantification (LOQ) and detection (LOD) were 0.4 μg/mL and 0.08 μg/mL for calycosin-7-O-β-D-glucoside, 0.2 μg/mL and 0.06 μg/mL for ononin, 0.4 μg/mL and 0.1 μg/mL for calycosin, 0.5 μg/mL and 0.1 μg/mL formonetion, respectively. The standard recoveries were in the range of 96.5%−104.7%. The developed method has successfully been used for the determination of four main flavonoids in Astragali Radix from various sources and can be used for identification, differentiation and quality evaluation of Astragali Radix.
近年来,我国很多地方的行政村村民自治“山穷水复疑无路”,自然村草根自治却是“柳暗花明又一村”。正是这种自治绩效的差异,催生了基层社会对于村民自治有效实现形式的崭新探索,广东省清远市就是着力通过村民自治重心下移复归自然村自治传统,推进行政与自治的适度分离,推进村民自治的性质复归与功能复位。本文研究发现,“清远改革”在取得了一定成效的同时,也面临着一系列亟待突破的瓶颈。清远实验能否达成预期的改革目标或许尚需更长时间检验,但清远实验至少为我国村民自治制度改革提供了一个探索的方向和路径选择。
以二氯甲烷为溶剂,采用加速溶剂萃取法提取千斤拔化学组分,用气相色谱-质谱(GC-MS)检测提取物化学组分,利用化学计量学组合方法得到提取物中各组分的色谱和质谱信息,通过利用各组分质谱信息和NIST标准质谱库相似度而获得定性分析结果,以总体积积分法和归一化法相对定量.结果表明,解析获得73个色谱峰,定性分析出54个组分,为总质量的89.41%.二氯甲烷提取物中主要组分为烯类和酚类等,其中长叶烯、香芹酚、杉木烯和橘烯含量依次最高.所得结果信息量多,定性定量准确度高,可为千斤拔的研究和质量控制提供依据.
以具体案例为参照,探析国内外发达地区政府决策咨询机制建设的现状、特征及启示,提炼出重大科技决策咨询机制建设的特点与重点,结合广东省政府决策咨询机制建设实际,提出完善广东省政府科技咨询机制的对策建议.
建立了可释放特定芳香胺的偶氮染料的测定方法.相对现有方法,在前处理过程中增加了酸碱处理步骤,显著提高了部分芳香胺的回收率.采用中等极性色谱柱,避免了假阳性情况出现.采用该方法,2,4-二氨基苯甲醚平均回收率为36%,邻甲苯胺和2,4-二氨基甲苯平均回收率分别为74%和63%,其他芳香胺平均回收率在85%~108%.
以连续流动分析仪分析滤嘴中截留主流烟气中的氰化氢含量,滤嘴萃取液过滤膜后直接进样.考察了萃取液体积、萃取方式和萃取时间等前处理对氰化氢分析的影响.结果表明,4支抽吸后的滤嘴用0.1 mol/L的NaOH取液,室温下振荡萃取30 min,过水系滤膜后直接进样分析,方程线性关系良好、回收率高、稳定性和精密度良好,可作为滤嘴截留氰化氢含量的检测方法.
完善政府决策咨询机制是我国推进政府决策科学化、民主化的重要任务。通过梳理发达国家和国内部分省市政府决策咨询机构设置、运行概况及其影响政府决策的方式,以广东省政府科学技术咨询委员会为考察对象,分析广东省政府科技决策咨询机制的现状与问题,并提出进一步完善的对策建议。
Objective: To systematically study the chemical components in the dichloromethane extracts of Radix Paeoniae Rubra obtained by accelerated solvent extraction( ASE). Methods: The chemical compositions were detected by GC- MS. After the overlapping chromatographic peaks,which were first treated with the roughness penalty smoothing method,were resolved into pure chromatograms and spectra by heuristic evolving latent projection( HELP),qualitative analysis was acquired by similarity search in NIST library with the pure mass spectrum of each component and the quantitative results were acquired by calculating the volume of total two- way response and the normalization method. Results: Totally,52 of the 71 separated components in the dichloromethane extracts of Radix Paeoniae Rubra were identified and quantified,which accounted for 86. 97% of the total content. The main components were acids,alcohols,esters and phenols. Benzoic acid,paeonol and o- methyl phenol showed the highest content sequentially. Conclusions: A simple and rapid method for a systematic study of the chemical composition in the dichloromethane extracts of Radix Paeoniae Rubra is developed. Not only more information is obtained,but also the qualitative analysis of components is improved to a reliable degree. The established method can provide foundation for a further development and quality control of Radix Paeoniae Rubra.
以二氯甲烷为溶剂,用加速溶剂萃取法提取独活化学成分后,用气相色谱-质谱(GC-MS)联用法分析测定,提出了独活二氯甲烷提取物化学成分的方法.结果表明,共分辨出67个色谱峰,鉴定出48种成分,占独活化学成分总质量的86.27%.主要组分为含氧物质、萜类、酮类和酯类,如4-甲氧基-6丙烯基-1,3苯并二噁茂和1-[3-3-甲氧基-5-羟苯基]-1,2,3,4-四甲基异喹啉.该方法可用于独活的进一步开发和质量控制.
A simple and rapid method for qualitative and quantitative determination of the volatile chemical constituents in Sichuan lovage rhizome was reported.The accelerated solvent extraction followed by gas chromatography-mass spectrometry and chemometric resolution methods was applied for the analysis.After the overlapping chromatographic peaks were resolved into pure chromatograms and spectra with subwindow factor analysis(SFA),qualitative analysis was performed by similarity search in NIST library with the obtained pure mass spectrum of each component and the quantitative results were obtained by calculating the volume of total two-way response.56of the 67separated constituents in essential oil of Sichuan lovage rhizome,which accounted for about 87.67% of the total content,were identified and quantified.The method is simple,fast and easy to be operated,and it can be used for the quality control of Sichuan lovage rhizome and other Chinese medicine.
Analysis of the volatile components in Agrimonia pilosa Ledeb with heuristic evolving latent projections (HELP) was presented. After extracted with water distillation method, the volatile components were detected by GCMS. Then the qualitative and quantitative analysis of the volatile components was completed with HELP resolving two-dimensional original data into mass spectra and chromatograms. 62 of 83 separated constituents in the total ion chromatogram of the volatile components were identified and quantified, accounting for about 86.49% of the total content. The obtained information can provide foundation for further study of Agrimonia pilosa Ledeb. This developed method can also be used for quality control of Agrimonia pilosa Ledeb samples.
The volatile chemical constituents in Agrimonla Pilosa Ledeb were extracted with steam distillation.Then they were detected and identified by chromatography-mass spectrometry(GC-MS)combined with Kovats retention indices(KI).The relative content of each component was determined by area normalization.A total of 67 components were detected and 48 main components were identified by MS combined with Kovats retention indices(KI),accounting for 87.35% of the total content.The components with high contents were as follows:cedrol(17.50%),α-pinene(11.60%),linalool(6.29%),α-terpineol(4.90%)and bornyl acetate(4.37%).The identified results of the volatile chemical constituents in Agrimonla pilosa Ledeb.by MS combined with Kovats retention indices(KI)were much more accurate.The established method can be used for further study of chemical constituents and quality control of Agrimonla pilosa Ledeb..
采用水蒸气蒸馏法从川赤芍中提取挥发油,用气相色谱/质谱联用法(GC/MS)检测并分析其化学成分,用归一化法测定其相对含量,结果鉴定出37个成分,占挥发油总成分的86.15%.主要成分为苯甲酸、牡丹酚和邻甲基苯酚.
Gas chromatography-mass spectrometry and multivariate curve resolution were applied to the differential analysis of the volatile components in Agrimonia eupatoria specimens from different plant parts. After extracted with water distillation method, the volatile components in Agrimonia eupatoria from leaves and roots were detected by GC-MS. Then the qualitative and quantitative analysis of the volatile components in the main root of Agrimonia eupatoria was completed with the help of subwindow factor analysis resolving two-dimensional original data into mass spectra and chromatograms. 68 of 87 separated constituents in the total ion chromatogram of the volatile components were identified and quantified, accounting for about 87.03% of the total content. Then, the common peaks in leaf were extracted with orthogonal projection resolution method. Among the components determined, there were 52 components coexisting in the studied samples although the relative content of each component showed difference to some extent. The results showed a fair consistency in their GC-MS fingerprint. It was the first time to apply orthogonal projection method to compare different plant parts of Agrimonia eupatoria , and it reduced the burden of qualitative analysis as well as the subjectivity. The obtained results proved the combined approach powerful for the analysis of complex Agrimonia eupatoria samples. The developed method can be used to further study and quality control of Agrimonia eupatoria .
A method for the study of the volatile components in Atractlodesm acrocephala Koidz from different sources with combined chemometrics methods was developed. After the volatile components in Atractlodesm acrocephala Koidz from two different locations were detected by GC MS, the qualitative and quantitative analysis of the volatile components of Atractlodesm acrocephala Koidz from Tiantai was conducted with SFA. Then, the common peak in Atractlodesm acrocephala Koidz sample from Xinan was extracted with orthogonal projection method. Among the identified components, there were 37 components coexisting in the studied samples although the relative content of each component showed difference to some extent. The obtained results can provide useful information for the developing of fingerprint of Atractlodesm acrocephala Koidz. It also can be used to compare the sameness and differences of Atractlodesm acrocephala Koidz from different sources and for quality control of Atractlodesm acrocephala Koidz.
Objective: To study the volatile chemical constituents in the dried shoots of Artemisia capillaris Thunb.Methods: The essential oil was extracted by steam distillation.The chemical compositions were detected by GC-MS.After the overlapping of chromatographic peaks,which were first treated with roughness penalty smoothing method,were resolved into pure chromatograms and spectra with subwindow factor analysis method(SFA),qualitative analysis was performed by similarity search in NIST library with the obtained pure mass spectrum of each component and the quantitative results were obtained by overall volume integration.Results: A total of 67 chromatographic peaks were separated,and 48 chemical components in the essential oil of the dried shoots of Artemisia capillaris Thunb.were identified,which accounted for 89.03% of the total content.The main components were n-hexadecanoic acid,9,12,15-octadecatrienoic acid,Artemisia capillaris falcarinol,trans-Z-alpha-bisabolene epoxide and germacrene D.Conclusions: Not only more components were identified by the established method,but also the accuracy of the qualitative analysis of components was improved.The established method can be used for further development and quality control of Artemisia capillaris Thunb.
目的 探讨实施持续性质量改进(CQI)管理模式对提高维持性血液透析(MHD)患者透析效果的影响.方法 观察实施CQI管理模式前后146名MHD患者血压控制、尿素清除指数(KT/V)、血管通路感染发生率、血管通路内瘘狭窄发生率等方面的变化.结果 实施CQI后,MHD患者的血压控制达标率由52.74%升至69.86%,KT/V达标率由78.77%上升至95.20%,血管通路感染发生率由5.48%降至1.37%,血管通路内瘘狭窄发生率由8.90%降至2.05%,与实施前比较,差异均有统计学意义(P<0.05).结论 实施CQI管理后MHD患者透析效果及质量明显改善.
The extracted volatile oils from Radix Angelecae pubescentis with water-steam distillation were detected,and the chemistry components were analyzed with GC-MS method.Then the relative contents were quantitatively determined by normalization method.39 components were identified,which accounted for 83.10%of the total volatile oil.The main components were 1, 3-benzodioxole,4-methoxy-6-(2-propenyl) and isoquinoline,l-[3-methoxy-5-hydroxybenzyl]-l,2,3, 4-tetramethyl.