高效液相色谱法检测食品中姜黄素类化合物

建立了食品中姜黄素类化合物的液相色谱分析方法。采用甲醇提取试样中姜黄素及其同系物去甲氧基姜黄素和双去甲氧基姜黄素,以YMCTMCarotenoid色谱柱(250 mm×4.6 mm,5μm)分离,甲醇水溶液(A)-甲基叔丁基醚(B)梯度洗脱。对所分析化合物的稳定性、前处理条件及色谱条件进行考察。3种分析物在0.5~100μg/mL范围内线性关系良好,相关系数为0.997 7~0.999 8。在10~100 mg/kg加标浓度范围内,平均回收率为72.2%~102%,相对标准偏差为3.4%~13.8%。对姜黄素、去甲氧基姜黄素和双去甲氧基姜黄素的检出限分别为6、5、5 mg/kg。方法稳定、可靠,已应用于实际样品的检测。     

反相高效液相色谱测定雷公藤浸膏中甲素的含量

报道了液固萃取-反相高效液相色谱法测定雷公藤浸膏(乙酸乙酯提取物)中甲素含量的方法。用LichrospherC18色谱柱，以甲醇：水-60：40(V／V)溶液为流动相，检测波长218nm。方法回收率为99．4％，变异系数为0．53％，方法快速，重现性及准确度能满足雷公藤浸膏中甲素含量测定的要求。     

HPLC法测定苦参碱阴道凝胶中的有关物质

用HPLC法测定苦参碱阴道凝胶中的有关物质，采用ODS色谱柱，以pH=4．0的0．25％(体积分数)磷酸缓冲溶液-三乙胺-乙腈(体积比为96：0．2：4)为流动相，流速为1．0mL／min，检测波长为210nm，苦参碱的浓度为0．786～1．834μg/mL时与色谱峰面积有良好的线性关系，相关系数为0．9994。有关物质含量测定结果稳定，相对标准偏差为2．33％。     

高效液相色谱法测定金羚感冒胶囊中阿司匹林的含量

用高效液相色谱法测定金羚感冒胶囊中阿司匹林的含量：采用RP-C18色谱柱,体积比为30：70的甲醇-0．03mol／L磷酸二氢钾溶液(用磷酸调节至pH=2．4)作流动相,流速为1．0mL／min,检测波长为280nm,阿司匹林色谱峰面积与其浓度在146.8～734μg／mL内线性关系良好,相关系数r=0．9998,阿司匹林的平均回收率为99．70％,相对标准偏差为0.18％(n=5)。     

高效液相色谱指纹图谱在中药芦根上的应用

利用现代分离分析技术如高效液相色谱(HPLC)与气相色谱(GC),能够获得中草药的色谱指纹图谱。本实验报道了高效液相指纹图谱应用于快速检测中草药提取物以及应用于研究、开发与生产中的质量控制体系中,利用HPLC建立芦根的色谱指纹图谱。实验条件为反相C18柱,流速为1．0mL／min,紫外检测器(λ=230nm)。通过分析比较色谱指纹图谱中的相对保留值α以及相对面积St对不同产地的芦根进行对比研究。这种基于HPLC的分析策略为中草药的精确鉴定和质量控制提供了有效的信息,并为HPLC在复杂组分样品中的应用开拓了新的领域。     

郁金药材中姜黄素类成分含量测定方法研究

开展了郁金药材中姜黄素类成分的含量测定的研究,确立了姜黄素的优化提取条件,建立了姜黄素的高效液相色谱含量测定方法。通过筛选,发现以60％乙醇回流,15倍药材溶剂量,提取时间1h,提取次数1次对姜黄素的提取较完全。姜黄素在0．0265～0．2648μg范围内线性关系良好。精密度、稳定性和重复性的RSD均小于2％,平均加标回收率为99。73％,RSD为1．41％。     

多功能柱净化-高效液相色谱法检测谷物中的玉米赤霉烯酮

建立了玉米和小麦中玉米赤霉烯酮（ZEN）的多功能柱净化-高效液相色谱检测方法。样品经乙腈-水混合溶剂（V（乙腈）：V（水）=84：16）提取，通过多功能净化柱（MFC）进行一次性净化，以Symmetry^R C18柱为分离柱，甲醇-水（V（甲醇）：V（水）=68：32）为流动相进行高效液相色谱分离和检测。玉米赤霉烯酮的质量浓度在0．01～4．0μg／mL范围内呈良好线性，相关系数为0．9996。检出限为0．04μg／g，在0、04—5．0mg／kg添加范围内的回收率为87．5％～98．6％，相对标准偏差为1．5％～8．3％。     

高效液相色谱法测定食品中的姜黄素

食品中的姜黄素经甲醇提取、净化后,以液相色谱-紫外检测器外标法定量检测.色谱条件:反相C<,18>色谱柱(250 mm x4.6 mm,5μm),以乙腈-0.05%乙酸氨水溶液为流动相等度洗脱,流速为1.0 mL/min.姜黄素质量浓度在0.5-50.0μg/mL范围内与峰面积呈线性关系,回归方程y=7440x-295...     

铅形态的高效液相色谱-电感耦合等离子体质谱分析

用50mm的反相高效液相色谱短柱在V甲醇/VH2O=55／45,其中水相为0．1mol／L乙酸0．1mol／L乙酸铵的缓冲溶液（pH=4．70）,流速0．6mL／min条件下,约10min内实现了无机铅离子（Pb^2＋）、氯化三甲基铅（TML）、氯化三乙基铅（TEL）和氯化三苯基铅（TPhL）的高效液相色谱．电感耦合等离子体质谱（HPLC-ICP-MS）联用分析。4种铅形态在去离子水和自来水中的加标回收率分别为93．8％-115．6％和89．3％-137．8％;峰强度和保留时间的RSD分别为7．4％-14．3％和0．5％-1．3％;仪器检出限及方法检出限分别为0．27-3．07μg/L和1．20-2．33μg／L。     

高效液相色谱法测定生姜中的6-姜酚

用C18色谱柱，以V(甲醇)：V(水)：V(冰乙酸)=35：64：1溶液作流动相，进样量5μL，在流速1．0mL／min下，可不经分离直接测定生姜中的6-姜酚。方法RSD小于1．00％，回收率97％～102％，相关系数0．9999。     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described.     

正丁胺对激光染料荧光谱影响的研究

用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在.     

Cu0-catalysed 1,3-dipolar cycloadditions of α-amino acid derived N,N-cyclic azomethine imines to ynones

A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu⁰ as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than Cu^I in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT).     

Synthesis and antioxidative/anti-inflammatory activity of novel fullerene–polyamine conjugates

(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C₆₀, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine.