One of the ultimate targets of array pattern synthesis is to maintain the mainbeam while suppressing the peak sidelode level (PSLL) within a smaller aperture size. The mainbeam gain proportionally increases with the aperture size, whereas the PSLL is uncorrelated approximately. This regular is useful for adjusting the array pattern as changing the aperture size. However, when the mutual coupling effect among the coupled array elements is considered, for some kinds of nonuniform arrays, e.g., the concentric ring array or the concentric elliptical array (CEA), the PSLL property would change significantly when the same array arrangement with different aperture sizes is used. On the purpose of both the PSLL suppression and the aperture reduction, this letter presents a pattern synthesis approach of real coupled CEAs. The form of elliptic ring is mainly introduced for the aperture reduction, and the ellipse-axis ratio, together with the ring radii and the position of each array element along the elliptic rings, are optimized simultaneously for the PSLL suppression. Typical examples are provided to validate the effectiveness of the synthesis approach. This approach also gives an alternative way for the adjustment of real coupled arrays after the theoretical synthesis.
采用顶空气相色谱-离子迁移谱(headspace-gas chromatography-ion mobility spectrometry,HS-GC-IMS)技术对云南不同品种生咖啡豆的挥发性有机物(volatile organic compounds,VOCs)进行无损分析.根据保留指数和迁移时间对其挥发性成分进行二维定性,创建生咖啡豆VOCs的差异谱图,并对其VOCs数据进行主成分分析(principal component analysis,PCA).结果 表明,HS-GC-IMS可有效分离生咖啡豆挥发性成分,对样品VOCs的信息采集及分析可在20 min内完成,并鉴定出42种挥发性物质,主要为醛类、酯类、醇类、酮类、吡嗪类、酸类及含硫化合物.采用PCA分析HS-GC-IMS图谱,可准确区分不同品种生咖啡豆.该方法具有快速、灵敏、无损的特点,为生咖啡豆的品种识别、产地追溯、品质控制等提供了一定参考依据和理论基础.
建立超高效液相色谱-串联质谱法同时快速检测辅助降血脂类保健食品中6种降血脂药物(烟酸、普伐他汀钠、氟伐他汀钠、美伐他汀、洛伐他汀、辛伐他汀)的方法.样品经甲醇提取,Waters Acquity BEH-C18色谱柱分离,0.1%甲酸-乙腈溶液梯度洗脱,流速0.2 mL/min,电喷雾离子源正离子模式扫描,多反应监测模式测定,外标法定量.结果表明:在实验条件下4 min内可快速、准确地定性定量分析6种降血脂化学药物,分离度良好,方法检出限为4~39μg/kg,加样回收率为80.2%~106.1%.利用本方法检测20批降血脂类保健食品,其中3批分别含有烟酸和洛伐他汀.本方法线性关系良好、快速、简便、准确,可作为辅助降血脂类保健食品中非法添加化学药物的定性定量检测方法.
The contents of hydrolytic amino acid and free amino acid of Maca from Huize areas of Yunnan were determined by RP-HPLC.Maca contained 18 kinds of amino acids.The percentage of human essential amino acid content of the total amino acid content was up to 36.75%.The results showed that Maca was a kind of high nutrient plant.Among human essential amino acids,the contents of Phe,Tyr,Mets and Cys were insufficient,which affected its nutritive value.Finally,the flavor of Maca was studied by the each flavor class amino acid in the free amino acid.
Zijuan tea is a rare special tea in Yunnan.In this paper,amino acids and trace elements of Zijuan tea with different processing methods(baked green tea,sun-dry tea,black tea and fermented Pu’er tea) were studied by using liquid chromatography with pre-column derivation.The content of trace elements(Cu,Zn,Fe and Mn) was analyzed by atomic absorption photometry.The results showed that there were differences in species and content of free amino acids in tea product with different processing methods.Analysis of score of ratio coefficient of amino acid showed that there were differences in nutritional value of free amino acids in the same tea materials with different processing methods.Little difference was found in the contents of trace elements Cu and Zn in Zijuan tea with different processing method.However,the contents of Fe and Mn were significantly varied in the different tea samples.
A high performance liquid chromatography(HPLC) method for fast qualitative analysis and accurately quantitative determination of artificial sweetener neotame in wine was developed.Neotame was qualitatively analyzed on a Waters Nova-Pak C18 column with an ultraviolet detector at 218 nm using acetonitrile: ion-pair reagent = 40:60(V/V) as the mobile phase,and the retention time of neotame was approximately 13.4 min.The contents of neotame in the suspected samples were determined under gradient elution condition,and the retention time of neotame was approximately 15.9 min.The detection limit of the developed method was 0.37 μg/mL,and the mean recovery rate for neotame in blank wine samples with spiked standard was 99%–101% with a relative standard deviation less than 1.0%(n = 5).This method is simple,accurate and practical,and can save 50% time during the analysis of large number of samples.
In this paper,the nutritional components was analyzed of Maca(Lepidium meyenii Walp)in the Lijiang planting area,It contains rich protein,carbohydrates,minerals,vitamins,fatty acids and amino acid etc. And through the test prove Maca polysaccharide in vitro has certain antioxidant health care function,For the success of manasseh were and further card provides the basis for the research and development.
A comparative analysis of the total flavones content in Panax notoginseng flowers from different areas was performed.The total flavones content in Panax notoginseng flowers was determined at 508nm by ultraviolet spectrophotometric with rutin as the reference substance.Based on the experiment of single factor,the optimum extraction conditions were as follow: ethanol concentration 60%,ratio of liquid to solid 1:25,extraction time 1h.Total flavones in Panax notoginseng flowers from different areas were compared and highest content was 0.73%,the lowest was only 0.43%.The repetition,stability and precision of the method in analyzing the total flavones content are promising.The method can be used to control the quality of Panax notoginseng flowers.
An HPLC–PDA fingerprint method has been developed for quality control of Panax notoginseng flowers. HPLC separation was performed at 35 °C on a Hypersil ODS column (4.6 mm × 250 mm, 5 μm); the mobile phase was an acetonitrile–water gradient at a flow rate of 1.0 mL/min. Satisfactory separation of 19 common peaks was achieved within 60 min. Similarity evaluation was performed by use of the professional software “Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine”, and the similarity among 12 batches of samples was no less than 0.93. Results of similarity evaluation confirmed that the quality of P. notoginseng flowers was stable, and that fingerprint analysis enabled precise and efficient quality control of P. notoginseng flowers.
The main bioactive constituents in Salvia yunnanensis C.H.Wright are rosmarinic acid,yunnaneic acid A-H and lithospermic acid etc.The chemical constituents and pharmacological effects of Salvia yunnanensis C.H.Wright were summarized in brief,and the results provided valuable reference for research and development.
Both oleanic acid and ursolic acid were separated on an RP C18 column.The mobile phase was acetonitrile-methanol-0.5% ammonium acetate(67∶12∶21).The detection wavelength was 210nm.The linear ranges were 0.0195—0.78μg for oleanic acid(r=0.9997)and 0.081—3.24μg for ursolic acid(r=0.9999).The recovery was 98.76% with RSD of 0.76% for oleanic acid and 99.04% with RSD of 0.80% for ursolic acid.The method is simple,rapid and accurate,and can be used for the quality control of shanzhajing jiangzhi tablets.
To establish an UPLC method in determination the amounts of Amino Acids in Walnuts.A Waters Acquity UPLC BEH C18 column(2.1 mm×150 mm,1.7μm)was applied,using AccQ.Tag Ultraa eluent A and AccQ.Tag Ultraa eluent B as the mobile phase,with a flow rate of 0.7 mL/min,and the column temperature 55℃.The calibration curve was linear in the range of 0.003~0.18 mg/mL of Amino Acids(r>0.999 4).The average recovery of Amino Acids was 98.5%.It has the advantage of simple,accuracy,and repeatable in the determination Amino Acids.
The method for the determination of the content of cyclophosphamide in human plasma was established by ultra performance liquid chromatography-mass spectrometry(UPLC/MS/MS)method.The samples were extracted by high-speed centrifugation and protein precipitation with methanol.The separation of cyclophosphamide was performed on Waters Acquity UPLC BEH C18 column(50mm×2.1mm,1.7μm) with the mobile phase of 0.1% ethanoic acid aqueous solution∶acetonitrile(80∶20) at a flow rate of 0.4mL·min-1,and that were determined by positive ESI MS/MS.The detection daughter ions of MS/MS were m/z 140.0 and 106.0 by external standard method.The calibration curves were good linear between the concentrations of 2—100ng·mL-1(r=0.9999).The limit of detection was 1μg·L-1.The recoveies of cyclophosphamide were in the range of 98.4%—100.5% and the RSD was less than 2.5%.This method is suitable for the study on clinical pharmacokinetics of cyclophosphamide.
分别以聚乙烯亚胺(PEI)、十六烷基三甲基溴化铵(CTMAB)对硅胶(SiO2)表面进行修饰,并以苯酚为模板,合成硅胶表面修饰分子印迹聚合物(MIP-SiO2),制备获得功能添加剂PEI-SiO2、CTMAB-SiO2、MIP-SiO2。按不同剂量分别将功能添加剂加入到卷烟滤嘴中,考察对卷烟主流烟气中苯酚的截留效率。结果表明,各添加剂均可有效降低卷烟烟气中的苯酚释放量。当添加量达到20mg/支时,各功能材料对苯酚的截留效率均超过39%。且添加剂对烟气中苯酚的截留能力大于对烟气中焦油的吸附能力,表明功能添加剂具有选择性降低卷烟烟气中苯酚的作用。
Ordered mesoporous carbons with high specific surface areas were prepared by evaporation induced triconstituent co-assembly method,with phenolic resin oligomers as organic precursor,tetraethyl orthosilicate(TEOS) as inorganic precursor and segmented copolymer F127 as template.The composition,structure and morphology of the prepared samples were characterized by XRD,TEM,FTIR,Raman and N2 sorption techniques.The prepared ordered mesoporous carbons had highly ordered two dimension-hexagonal mesostructured with the average aperture of 6.5nm,and the specific surface area and pore volume reached up to 2281m2/g and 1.92cm3/g,respectively.
The method for the determination of the residues of metsulfuron-methyl and bensulfuron-methyl in soil was established by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).The residues of metsulfuron-methyl and bensulfuron-methyl were extracted with solid phase extraction C18,and the separation of metsulfuron-methyl and bensulfuron-methyl were performed on Waters Acquity UPLC system with a BEH C18 column(50mm×2.1mm,1.7μm) with a linear gradient elution(methyl alcohol:0.05% acetic acid as mobile phase) at a flow rate of 0.4mL·min-1,and that were detected by MS/MS with positive electrospray ionization mode.The methods were quantified by external standard method.The calibration curves were good linear between the concentrations of 1.0—100.0μg·L-1,and correlation coefficients(r) were 0.9997 and 0.9999 for metsulfuron-methyl and bensulfuron-methyl,respectively.The detection limits for metsulfuron-methyl and bensulfuron-methyl were 0.02μg·kg-1 and 0.03μg·kg-1,respectively,and the recoveries were in the range of 86.2%—96.5% with the RSD not more than 5.1%.This method is proved to be simple,fast,reliable and accurate.
AIM To develop an HPLC method for determing sodium danshensu,protocate chuicaldehyde,caffeic acid,cryptotanshinone,tanshinoneⅠ and tanshinone ⅡA simultaneously in Salvia yunnanensis Roots.METHODS The column was Hypersil ODS(4.6 mm × 250 mm,5μm).The mobile phase consisted of acetonitrile(A) -water(containing 0.1% phosphoric acid)(B) in the gradient mode.The flow-rate was 1.0 mL/min.The detecting wave length was set at 280 nm.RESULTS The relationship between the concentration and the peak areas of the six compounds was all linear.The RSD of recovery were all less than 3.0%.CONCLUSION The method is simple,rapid and accurate and reproducible,and could be used for the quality control of Salvia yunnanensis C.H.Wright.
A new 1-naphthalenamine(NNA) specific molecularly imprinted polymer(MIP) was synthesized based on non-covalent interaction.The molecular recognition characteristics of the template polymer were evaluated by UV,IR,XPS and 1H NMR.The NNA-MAA complexes of 1∶1 mole ratio were obtained by nitrogen bonding and the complexes possessed better stabilization(K=5.537×104L/mol).Furthermore,hydrogen atom of the amino group in 1-naphthalenamine is hydrogen-bond acceptors.Hydrogen atom of the lactam group in methacrylic acid is hydrogen-bond donor,being the predominant binding sites interacting with 1-naphthalenamine.The adsorption characteristics of MIP was evaluated by equilibrium adsorption experiment.The results indicate that MIP performs highly selectivity to 1-naphthalenamine.
A method for determination of the amounts of amino acids in tobacco by UPLC was established.A Waters Acquity UPLC BEH C18 column(2.1mm×100mm,1.7μm)was applied,using AccQ.Tag Ultraa Eluent A and AccQ.Tag Ultraa Eluent B as mobile phase,with a flow rate of 0.7mL·min-1,and the wavelength was 248nm,the column temperature was 55℃.The calibration curve was linear in the range of 0.0030—0.204mg/mL of amino acids(r0.9994).The average recovery of amino acids was 98.7%.This method has the advantages of rapidity and accurate,repeatability in determination of amino acids in tobacco in ten minutes.
A method for simultaneous determination of baicalin,chlorogenic acid and rutin in the yin huang buccal tablets was developed.A hypersil ODS C18(4.6mm×200mm,5μm) column was used.A mixture of methanol-water-acetic acid(10:88:2)was used as mobile phase A and the mixture of methanol-water-acetic acid(88:10:2) as mobile phase B.Phase A-phase B in gradient elution:0 min (97:3)-10min(73:27)-25min(20:80)-36min(20:80) at a flow rate of 1.0mL/min.The detection wavelength was set at 327 nm and 280 nm and the column temperature was 25℃.The calibration curve was linear in the range of 0.051—0.512μg/mL for baicalin(r=0.9990),average recovery was 98.23% and RSD was 2.13% (n=6).The calibration curve was linear in a range of 0.059—0.592μg/mL for chlorogenic acid(r=0.9996),average recovery was 97.61% and RSD was 2.13%(n=6).The calibration curve was linear in a range of 0.087—0.868μg/mL for rutin(r=0.9992),average recovery was 98.56% and RSD was 1.13%(n=6).The method is sensitive,reproducible,and suitable for the quality control of the yin huang buccal tablets.