RESUMO
To reveal the processing mechanism of Chrysanthemi Flos from the changes of chemical compositions after frying and its effect on the efficacy of liver protection. Ultra performance liquid chromatography-quadrupole-time of flight-mass spectrometry(UPLC-Q-TOF-MS) and ultra high performance liquid chromatography(HPLC) were used for the qualitative and quantitative researches of chemical compositions before and after Chrysanthemi Flos frying. Progenesis QI and SPSS software were used for principal component analysis(PCA), partial least squares discriminant analysis(PLS-DA), variable importance projection(VIP) analysis and t-test to identify the compositions with significant changes. Pharmacodynamics experiment was used to investigate the protective effect of crude and fried Chrysanthemi Flos on CCl_4-induced acute liver injury in mice. According to mass spectrometry data, there were 28 chemical compositions in crude and fried Chrysanthemi Flos, mainly including flavonoids and organic acids. 13 compositions such as luteolin, apigenin and luteolin glycoside were increased significantly after frying, while 7 compositions such as chlorogenic acid, luteolin-7-O-glucuronide and apigenin-7-O-glucuronide were decreased significantly after frying. Through principal component analysis, crude and fried Chrysanthemi Flos products were divided into two categories, indicating that there were internal differences in quality. The results of liver injury protection experiment in mice showed that the AST, ALT and MDA contents were significantly decreased and SOD level was increased in mice with liver injury in both the high and medium dose groups. Histopathological examination showed that crude and fried Chrysanthemi Flos can protect the liver by reducing inflammatory cell infiltration, reducing steatosis, and repairing damaged liver cells. The results of this study showed that the chemical compositions had obvious changes after frying, and both crude and fried Chrysanthemis Flos had protective effects on CCl_4-induced acute liver injury in mice. In addition, in the range of high, medium and low doses, the liver protection effect of crude and fried Chrysanthemi Flos increased with the increase of dose. The experiment results provided reference for the mechanism of fried Chrysanthemi Flos and clinical selection of processed products.
Assuntos
Chrysanthemum , Animais , Cromatografia Líquida de Alta Pressão , Flavonoides/análise , Flores/química , Fígado/química , CamundongosRESUMO
BACKGROUND: Dioscorea is a genus of flowering plants, and some Dioscorea species are known and used as a source for the steroidal sapogenin diosgenin. To screen potential resource from Dioscorea species and related medicinal plants for diosgenin extraction, a rapid method to compare the contents of diosgenin in various plants is crucial. RESULTS: An ultra-performance liquid chromatography (UPLC) coupled with diode array detection (DAD) and electrospray ionization mass spectrometry (ESI-MS) method was developed for identification and determination of diosgenin in various plants. A comprehensive validation of the developed method was conducted. Twenty-four batches of plant samples from four Dioscorea species, one Smilax species and two Heterosmilax species were analyzed by using the developed method.The present method presented good sensitivity, precision and accuracy. Diosgenin was found in three Dioscorea species and one Heterosmilax species, namely D. zingiberensis, D. septemloba, D. collettii and H. yunnanensis. CONCLUSION: The method is suitable for the screening of diosgenin resources from plants. D. zingiberensis is an important resource for diosgenin harvesting.
Assuntos
Técnicas de Química Analítica , Dioscorea , Diosgenina/análise , Extratos Vegetais/química , Smilax , China , Cromatografia Líquida de Alta Pressão , Estudos de Viabilidade , Medicina Herbária/métodos , Humanos , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Espectrometria de Massas por Ionização por Electrospray , Raios UltravioletaRESUMO
BACKGROUND: Fish oil is a popular nutritional product consumed in Hong Kong. Eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) are the two main bioactive components responsible for the health benefits of fish oil. Market survey in Hong Kong demonstrated that various fish oil capsules with different origins and prices are sold simultaneously. However, these capsules are labelled with same ingredient levels, namely EPA 180 mg/g and DHA 120 mg/g. This situation makes the consumers very confused. To evaluate the quality of various fish oil capsules, a comparative analysis of the contents of EPA and DHA in fish oil is crucial. METHODS: A gas chromatography-mass spectrometry (GC-MS) method was developed for identification and determination of EPA and DHA in fish oil capsules. A comprehensive validation of the developed method was conducted. Ten batches of fish oil capsules samples purchased from drugstores of Hong Kong were analyzed by using the developed method. RESULTS: The present method presented good sensitivity, precision and accuracy. The limits of detection (LOD) for EPA and DHA were 0.08 ng and 0.21 ng, respectively. The relative standard deviation (RSD) values of EPA and DHA for repeatability tests were both less than 1.05%; and the recovery for accuracy test of EPA and DHA were 100.50% and 103.83%, respectively. In ten fish oil samples, the contents of EPA ranged from 39.52 mg/g to 509.16 mg/g, and the contents of DHA ranged from 35.14 mg/g to 645.70 mg/g. CONCLUSION: The present method is suitable for the quantitative analysis of EPA and DHA in fish oil capsules. There is a significant variation in the contents of the quantified components in fish oil samples, and there is not a linear relationship between price and contents of EPA and DHA. Strict supervision of the labelling of the fish oil capsules is urgently needed.
Assuntos
Suplementos Nutricionais/análise , Ácidos Docosa-Hexaenoicos/análise , Ácido Eicosapentaenoico/análise , Óleos de Peixe/análise , Animais , Cápsulas , Cromatografia Gasosa-Espectrometria de Massas , HumanosRESUMO
OBJECTIVE: To compare the contents of four alkaloids and antitussive activities of Stemona tuberosa from different habitats of Guangxi Province. METHODS: The HPLC separation was performed on a Merck Purospher STAR RP18 (250 mm x 4. 6 mm, 5 µm) column by gradient elution using 0. 05% ammonia-acetonitrile as the mobile phase. The flow rate was 1. 0 mL/min, the dectection wave-length was set at 210 nm,and the column temperature was 40 °C. The antitussive potency of total alkaloids of Stemonae Radix from different habitats was evaluated on guinea pigs with citric acid aerosol to induce cough. RESULTS: The range of recoveries of this mehtod was 98. 24% ~ 101. 21%, with all the constituents showing good linearity(the correlation coefficents above 0. 999). The major chemotype of Stemonae Radix in Guangxi was stemoninine, following by tuberostemonine and croomine, and finally neotuberostemonine. The antitussive activitiy of Stemona tuberosa was in a concentration-dependent manner. CONCLUSION: Stemonae Radix from Dongxing, Fangcheng can reduce cough times and prolong cough incubation period, and thus Dongxing, Fangcheng is the best habitat in Guangxi in the present experiments.
Assuntos
Alcaloides/farmacologia , Antitussígenos/farmacologia , Medicamentos de Ervas Chinesas/farmacologia , Ecossistema , Stemonaceae/química , Alcaloides/isolamento & purificação , Animais , Antitussígenos/isolamento & purificação , China , Cromatografia Líquida de Alta Pressão , Tosse/tratamento farmacológico , Cobaias , Compostos Heterocíclicos com 3 Anéis , Lactonas , Raízes de Plantas/química , Pirrolidinas , Compostos de EspiroRESUMO
In this article, reversal activities of Euphorbia factor L1 (EFL1) against ABCB1-mediated multidrug resistance (MDR) and apoptosis sensitization in K562/ADR cells are reported. EFL1 decreased the IC50 values of anticancer agents in K562/ADR cells over-expressing ABCB1. However, EFL1 did not affect the IC50 values of anticancer agents in sensitive K562 cells. Additionally, EFL1 increased the intracellular accumulation of rhodamine 123 and doxorubicin in K562/ADR cells without affecting their accumulation in K562 cells. Furthermore, EFL1 sensitized the apoptosis triggered by vincristine in K562/ADR cells via mitochondrial pathway, as confirmed by Annexin V-FITC/PI detection and western blot. At the same time, EFL1 did not influence the apoptosis induced by vincristine in K562 cells. Western blot results showed that EFL1 did not affect the phosphorylation level of AKT and ERK in K562 and K562/ADR cells. Finally, EFL1 did not down-regulate protein expression of ABCB1.
Assuntos
Membro 1 da Subfamília B de Cassetes de Ligação de ATP/fisiologia , Antineoplásicos/farmacologia , Apoptose/efeitos dos fármacos , Diterpenos/farmacologia , Resistencia a Medicamentos Antineoplásicos/efeitos dos fármacos , Fenilpropionatos/farmacologia , Subfamília B de Transportador de Cassetes de Ligação de ATP , Caspases/metabolismo , Sobrevivência Celular/efeitos dos fármacos , Doxorrubicina/farmacologia , Resistência a Múltiplos Medicamentos/efeitos dos fármacos , Ensaios de Seleção de Medicamentos Antitumorais , Sinergismo Farmacológico , MAP Quinases Reguladas por Sinal Extracelular/metabolismo , Expressão Gênica , Humanos , Concentração Inibidora 50 , Células K562 , Fosforilação , Processamento de Proteína Pós-Traducional , Proteínas Proto-Oncogênicas c-akt/metabolismo , Vincristina/farmacologiaRESUMO
Fordiae Cauliflorae Radix (FC, the root of Fordia cauliflora Hemsl) and Millettiae Pulchrae Radix [MP, the root of Millettia pulchra (Benth.) Kurz var. laxior (Dunn) Z. Wei], which go under the same local name of "Daluosan", have long been used in Southern China for the treatment of stroke, paralysis, dementia in children, Alzheimer's disease and other diseases. The same local name and similar functions always confuse users. To further utilize these two ethnodrugs and identify them unambiguously, an HPLC-DAD-ESI-IT-TOF-MSn method was developed to separate and characterize the flavonoids in FC and MP. A total of 41 flavonoids were detected, of which six compounds were identified by comparing their retention time and MS data with those of the reference standards, and the others were tentatively identified based on their tandem mass spectrometry data obtained in the positive ion detection mode. Nineteen of these characterized compounds are reported from these two plants for the first time.
Assuntos
Fabaceae/química , Flavonoides/química , Chalcona/química , Cromatografia Líquida de Alta Pressão , Millettia/química , Estrutura Molecular , Raízes de Plantas/química , Espectrometria de Massas em TandemRESUMO
Rubus chingii var. suavissimus (S. K. Lee) L. T. Lu (RS)-a sweet plant also known as Tiancha distributed in the south of China where it is used as a beverage-recently gained extensive attention as adjuvant therapy of diabetes and hypertension. Although pharmacological studies indicate that RS has beneficial effects in regulating lipid metabolism disorder characteristics, the active chemicals responsible for this effect remains unclear. The present study aims to predict the effective substances of RS on regulating lipid metabolism disorder through the analysis of the chemical profile of RS, the absorbed prototype components in rat plasma, and network pharmacology. Also, a UPLC method able to quantify the screened potential effective chemicals of RS products was established. First, a total of 69 components-including diterpene, triterpenoids, flavonoids, polyphenols, and lignans-were systematically characterized in RS. Of those, 50 compounds were detected in the plasma of rats administered with RS extract. Through network pharmacology, 9 potential effective components, 71 target genes, and 20 pathways were predicted to be involved in RS-mediated regulation of lipid metabolism disorder. The quantitative analysis suggested that the contents of potential effective components varied among samples from different marketplaces. In conclusion, the presented results provide a chemical basis for further research of Rubus chingii var. suavissimus.
RESUMO
While the underlying mechanism remains unknown, Rubus chingii var. suavissimus (S. K. Lee) L. T. Lu or Rubus suavissimus S. Lee (RS), a sweet plant distributed in southwest of China, has been used as beverage and folk medicine. Pharmacological studies indicated the potential of RS improving the obesity phenotype and hyperlipidemia. The mechanism is still not yet to be put forward. To verify the substantial effects of RS on lipid metabolism, a Syrian golden hamster model was adopted. The physiological and pathological evaluation of experimental animals demonstrated that RS can relieve the lipid metabolism disorder induced by high-fat diet and alleviated liver injury. RS upregulation the expressions of peroxisome proliferator-activated receptor α (PPARα), PPARγ and CCAAT/enhancer binding protein α (C/EBPα), as well as adipocyte-specific genes, glucose transporter 4 (Glut4), lipoprotein lipase (LPL) and fatty acid binding protein 4 (aP2). On the other side, RS suppressed the sterol regulatory element binding protein 1 (SREBP1) and downstream acetyl-CoA carboxylase 1 (ACC1), stearoyl-CoA desaturase-1 (SCD1) and fatty acid synthase (FAS). In conclusion, RS alleviated lipid metabolism disorder symptoms caused by high-fat diet accompanied with 8 weeks of treatment, involving enhanced ß-oxidation, increased adipogenesis and decreased the metabolism of fatty acids, via modulation of the PPARs/SREBP pathway in Syrian golden hamsters.
Assuntos
Hiperlipidemias , Rubus , Animais , Cricetinae , Dieta Hiperlipídica/efeitos adversos , Metabolismo dos Lipídeos , Mesocricetus , PPAR gama/metabolismo , Proteína de Ligação a Elemento Regulador de Esterol 1/genéticaRESUMO
Stemona sessilifolia, S. japonica and S. tuberosa are the three genuine sources of Stemonae Radix specified in the Chinese Pharmacopoeia (CP) for antitussive and insecticidal remedy. Significant variations in alkaloids composition and content, as well as different degree of antitussive activity were found among them. In order to accurately identify the genuine sources of Stemonae Radix in the genetic level, two polymerase chain reaction-restriction fragment length polymorphism (PCR-RFLP) methods were developed based on the sequence differences in chloroplast DNA trnL-trnF and petB-petD regions of the species recorded in CP, as well as S. parviflora and a counterfeit of Stemonae Radix, Asparagus cochinchinensis. By using the restriction enzymes MwoI, AciI and XmnI which were able to recognize specific sequence sites in the trnL-trnF region, and BclI, HincII and BslI which can recognize those in the petB-petD region to digest the corresponding PCR products, the specific digestion pattern enabled the discrimination of the botanical sources of Stemonae Radix effectively and efficiently.
Assuntos
Primers do DNA/genética , DNA de Plantas/genética , Raízes de Plantas/genética , Reação em Cadeia da Polimerase/métodos , Polimorfismo de Fragmento de Restrição/genética , Stemonaceae/genética , Medicamentos de Ervas Chinesas , Folhas de Planta/genéticaRESUMO
Stemona sessilifolia, S. japonica and S. tuberosa are the three original sources of Stemonae Radix specified in the Chinese Pharmacopoeia (CP), and have been traditionally used for antitussive and insecticidal remedy. Significant variations in alkaloids composition and content, as well as different degrees of antitussive activities were found among them. In order to identify the genuine sources of Stemonae Radix accurately in genetic level, we determined the nucleotide sequences of chloroplast DNA trnL-trnF, trnH-psbA, petB-petD and trnK-rps16 regions of the species recorded in CP and S. parviflora, as well as the common counterfeits of Stemonae Radix, Asparagus species. The results revealed that the sequences of petB-petD and trnK-rps16 regions, showing relatively high substitution rate, were more informative than those of trnL-trnF and trnH-psbA regions. The sequences from all the four regions provided useful information to discriminate the three CP species from each other and from S. parviflora and the counterfeits. A phylogenetic tree reconstructed by the trnH-psbA sequences for 9 Stemona species distributed in China and Thailand showed that the three CP species belonged to the same clade, among which S. japonica and S. sessillifolia formed a sister group, showing closer relations to each other than to S. tuberosa. By contrast, S. parviflora was genetically far from the three CP species. Intra-species variations were observed in the three CP species. Especially, in S. tuberosa two types of petB-petD sequence and four types each of trnL-trnF, trnK-rps16 and trnH-psbA sequences resulted in 6 haplotypes; whereas, these differences had no relation with the different chemical types, but seemed to be consistent with geographical distribution.
Assuntos
DNA de Cloroplastos/genética , Medicina Tradicional Chinesa , Plantas Medicinais/genética , Stemonaceae/genética , Sequência de Bases , China , Dados de Sequência Molecular , Filogenia , Folhas de Planta/genética , Plantas Medicinais/crescimento & desenvolvimento , Reação em Cadeia da Polimerase , Stemonaceae/crescimento & desenvolvimentoRESUMO
A high-performance liquid chromatographic (HPLC) method was developed for the simultaneous quantification of five major bioactive constituents in the stems of resiniferous Dracaena plants from China and Vietnam, as well as those in the related traditional Chinese medicinal preparations. A diode array detector with the wavelength of 330 nm was used to monitor resveratrol, 7,4'-dihydroxyflavone and pterostilbene, while loureirin A and loureirin B were monitored at 280 nm. The five constituents were separated on an Agela SB C(18) column by gradient elution using 0.008% (v/v) formic acid solution (A) and acetonitrile (B) as the mobile phase. The validation of the method included recovery, linearity, accuracy and precision (intra- and inter-day variation). The range of recoveries of this method was 98.1-104.9%, with all the constituents showing good linearity (r(2) > 0.9999). The accuracy and precision were satisfactory, with the overall intra- and inter-day variation being less than 4%. The present method has been successfully applied for the determination of all five constituents in 21 related herbal samples including 10 D. cochinchinensis stem samples, seven D. cambodiana stem samples and four purchased medicinal preparations. The contents of these constituents were analyzed using principal component analysis, which can efficiently identify raw herb of Dracaena from different sources. The study may be considered helpful to the quality control of Dracena plants and its medicinal preparations.
Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Dracaena/química , Medicamentos de Ervas Chinesas/química , Extratos Vegetais/química , Preparações de Plantas/química , Caules de Planta/química , Plantas Medicinais/química , China , Extratos Vegetais/análise , Preparações de Plantas/análise , Análise de Componente Principal , Controle de Qualidade , VietnãRESUMO
OBJECTIVE: To study the anatomy of Dracaena cochinchinensis systematically, and find out the distribution and detect the constituents of its resin, in order to provide substantial foundation for the formation mechanism of its red resin. METHOD: The microscopic structures of D. cochinchinensis were systematically observed by using color micrographics, including stem with and without resin, roots, barks and leaves. The HPLC fingerprints of the stem with and without resin were compared. RESULT: Characteristics of the tangentical longitudinal section of stem with resin and surface view of leaves were elucidated. Besides xylem vessels and fibers of the stem, it was found that the red resin also exists in the cortex parenchyma cells of the stem and the medulla and xylem of the root. According to the HPLC fingerprint analysis result of the stems with and without resin, a number of flavones and stilbenoids were detected in the stem in which resin appeared after it wounded. CONCLUSION: No secretory tissue to secrete resin was found in D. cochinchinensis, further study is needed to elucidate the formation mechanism of its resin.
Assuntos
Dracaena/anatomia & histologia , Plantas Medicinais/anatomia & histologia , Resinas Vegetais/química , Dracaena/química , Dracaena/metabolismo , Plantas Medicinais/química , Plantas Medicinais/metabolismo , Resinas Vegetais/metabolismoRESUMO
The dried root tubers of Stemona tuberosa, S. japonica and S. sessilifolia are the original sources of Stemonae Radix (SR) for antitussive and insecticidal activities. The products of SR which are available on the market are variable, and imitations exist. In order to characterize the overall chemical constituents of SR and evaluate its quality, a novel, binary high-performance liquid chromatographic fingerprinting method, describing the pattern of alkaloids (fingerprint I) and non-alkaloids (fingerprint II) of SR was developed. It was also applied to determine whether the medicinal parts and the processing methods affect the quality of SR. Similarity and high-performance liquid chromatography-mass spectrometry (HPLC-MS(n)) were utilized to compare or identify the chemical constituents of SR. The results indicate that the chemical constituents from different parts of the underground material of Stemona plants are diverse and that the processing methods affect certain constituents in the root tuber samples. The similarity and the resulting chemical consitituents obtained show that the binary chromatographic fingerprint method can be used to differentiate the three official Stemona species or the adulterants of SR, which is helpful for the identification and quality evaluation of SR.
Assuntos
Medicamentos de Ervas Chinesas/química , Stemonaceae/química , Alcaloides/química , Alcaloides/isolamento & purificação , Cromatografia Líquida de Alta Pressão , Medicamentos de Ervas Chinesas/isolamento & purificação , Tubérculos/química , Espectrometria de Massas por Ionização por ElectrosprayRESUMO
ETHNOPHARMACOLOGICAL RELEVANCE: Saussurea involucrata Matsum. & Koidz. is an endangered species of the Asteraceae family, growing in the high mountains of central Asia. It has been, and is, widely used in traditional Uyghur, Mongolian and Kazakhstan medicine as well as in Traditional Chinese Medicine as Tianshan Snow Lotus (Chinese: ). In traditional medical theory, S. involucrata can promote blood circulation, thereby alleviating all symptoms associated with poor circulation. It also reputedly eliminates cold and dampness from the body, diminishes inflammation, invigorates, and strengthens Yin and Yang. It has long been used to treat rheumatoid arthritis, cough with cold, stomach ache, dysmenorrhea, and altitude sickness in Uyghur and Chinese medicine. AIM OF THE REVIEW: To comprehensively summarize the miscellaneous research that has been done regarding the botany, ethnopharmacology, phytochemistry, biological activity, and toxicology of S. involucrata. METHOD: An extensive review of the literature was carried out. Apart from different electronic databases including SciFinder, Chinese National Knowledge Infrastructure (CNKI), ScienceDirect that were sourced for information, abstracts, full-text articles and books written in English and Chinese, including those traditional records tracing back to the Qing Dynasty. Pharmacopoeia of China and other local herbal records in Uighur, Mongolian and Kazakhstan ethnomedicines were investigated and compared for pertinent information. RESULTS: The phytochemistry of S. involucrata has been comprehensively investigated. More than 70 compounds have been isolated and identified; they include phenylpropanoids, flavonoids, coumarins, lignans, sesquiterpenes, steroids, ceramides, polysaccharides. Scientific studies on the biological activity of S. involucrata are equally numerous. The herb has been shown to have anti-neoplastic, anti-inflammatory, analgesic, anti-oxidative, anti-fatigue, anti-aging, anti-hypoxic, neuroprotective and immunomodulating effects. Many have shown correlations to the traditional clinical applications in Traditional Chinese Medicine and medicines. The possible mechanisms of S. involucrata in treating various cancers are revealed in the article, these include inhibition of cancer cells by affecting their growth, adhesion, migration, aggregation and invasion, inhibition of epidermal growth factor receptor signaling in cancer cells, hindrance of cancer cell proliferation, causing cytotoxicity to cancer cells and promoting expression of tumor suppressor genes. Dosage efficacy is found to be generally concentration- and time-dependent. However, studies on the correlation between particular chemical constituents and specific bioactivities are limited. CONCLUSION: In this review, we have documented the existing traditional uses of S. involucrata and summarized recent research into the phytochemistry and pharmacology of S. involucrata. Many of the traditional uses have been validated by phytochemical and modern pharmacological studies but there are still some areas where the current knowledge could be improved. Although studies have confirmed that S. involucrata has a broad range of bioactivities, further in-depth studies on the exact bioactive molecules and the mechanism of action are expected. Whether we should use this herb independently or in combination deserves to be clarified. The exact quality control as well as the toxicology studies is necessary to guarantee the stability and safety of the clinic use. The sustainable use of this endangered resource was also addressed. In conclusion, this review was anticipated to highlight the importance of S. involucrata and provides some directions for the future development of this plant.
Assuntos
Medicamentos de Ervas Chinesas/química , Medicamentos de Ervas Chinesas/farmacologia , Extratos Vegetais/química , Extratos Vegetais/uso terapêutico , Saussurea/química , Animais , Medicamentos de Ervas Chinesas/efeitos adversos , Medicamentos de Ervas Chinesas/uso terapêutico , Etnofarmacologia , Humanos , Extratos Vegetais/efeitos adversos , Extratos Vegetais/farmacologiaRESUMO
Solvothermal reactions of mixed ligands H(3)BTC and macrocyclic oxamide complexes (ML, M = Cu, Ni) with M(ClO(4))(2)·6H(2)O (M = Co, Zn, Ni and Cd) afford six new complexes, including [M'(4)(BTC)(2)(ML)(2)(OH)(2)(H(2)O)(2)]·2H(2)O (M' = Co, M = Ni, for (1); M' = Zn, M = Ni, for (2); M' = Zn, M = Cu, for (3)), [Ni(3)(BTC)(2)(NiL)(2)(H(2)O)(6)]·2CH(3)OH·2H(2)O (4), [Cd(4)(BTC)(2)(HBTC)(NiL)(4)(H(2)O)]·3H(2)O (5) and [Cd(HBTC)(CuL)]·H(2)O (6) (ML, H(2)L = 2, 3-dioxo-5, 6, 14, 15-dibenzo-1,4,8,12-tetraazacyclo-pentadeca-7,13-dien; H(3)BTC = 1,3,5-benzenetricarboxylic acid). Complexes 1-3 consist of a 2D layer framework formed by the linkage of M(II)(M = Ni, Cu) and M'(4) (M' = Co, Zn) cluster via the oxamide and BTC(3-) bridges and display a (3,6)-connected network with a (4(3))(2)(4(6).6(6).8(3)) topology. The structure of 4 consists of pentanuclear [Ni(II)(5)] units and arranges in a 1D cluster chain. Complex 5 exhibits a 2D layered structure characterized by 3,4,3-connected (4.6(2))(3)(4.6(3).8(2))(4(2).6(3).8)(4(2).6) topology. Complex 6 possesses a 3D network with sra topology. The magnetic properties of complexes 1 and 4 were investigated.
RESUMO
Hydrothermal reactions of mixed ligands 5-sulfosalicylic acid (H(3)SSAL) and macrocyclic oxamide complex (CuL) with M(ClO(4))(2)·6H(2)O (M = Mn, Gd and Cu) afford three new complexes, including [Mn(II)(2)Mn(III)(SSAL)(2)(CuL)(2)(OH)(H(2)O)(3)]n (1), {[Gd(2)(HSSAL)(2)(CuL)(4)(C(2)O(4))(H(2)O)(2)]·2H(2)O}(n) (2) and [Cu(2)(HSSAL)(2)(CuL)(4)]·2H(2)O (3) (CuL, H(2)L = 2,3-dioxo-5,6,14,15-dibenzo-1,4,8,12-tetraazacyclo-pentadeca-7,13-diene). Complex 1 has very interesting mixed-valence manganese-copper Cu(II)Mn(II)Mn(III)Mn(II)Cu(II) units and consists of a 1D ladderlike chain formed by the linkage of copper(ii) and Mn(3) clusters via the oxamide and SSAL(3-) bridges. The structure of 2 consists of hexanuclear Cu(II)(4)Gd(III)(2) molecules and is arranged in a 1D ladderlike chain formed by the linkage of copper(ii) and gadolinium(iii) via the oxamide, oxalate and HSSAL(2-) bridges. Complex 3 is a hexanuclear Cu(II)(6) molecule including both oxamide and HSSAL(2-) bridges. The results of magnetic determination show pronounced antiferromagnetic interactions in 1 and 3, and ferromagnetic interactions in 2.