The determination of benzo[a]pyrene in the total particulate matter of cigarette smoke

A procedure for the isolation and determination of benzo[a]pyrene in the total particulate matter of cigarette smoke is described. Two high-pressure liquid chromatographic (HPLC) techniques are employed: a normal-phase, mu Bondapak-NH2, amino column is used for isolation of the benzo[a]pyrene fraction and a reversed-phase, Vydac 201TP54, polymeric octadecyl silane column is used for quantitation. Fluorescence detection is used in both modes of chromatography. The wavelengths of excitation and emission are evaluated for analytical detection. Extraction media and various isolation techniques are compared for their extraction efficiency and isolation from interferences, respectively. The procedure is efficient, reproducible, sensitive (3 pg), and gives results that compare favorably with other techniques reported in the literature for the B[a]P content of reference cigarettes, 1R1 and 1R4F.     

Clay Catalysis: Stork's Alkylation and Acylation of Cyclohexanone Without Isolation of Enamine

Cyclohexanone and morpholine in the presence of KSF under azeotropic distillation gave 1-morpholinocyclohexene which is alkylated or acylated in situ without isolation of the enamine. The overall yield of these Stork's reactions are better or equivalent to those obtained by isolation of the enamine.     

皂甙分离和结构鉴定研究进展

本文对近十年来皂甙分离方法和结构签定技术进行了综述，尤其是对HPLC及1DNMR、2DNMR各种新技术在皂甙分离和结构鉴定方面的应用，作了较为详细的总结。     

CAD-45大孔吸附树脂提取分离麦迪霉素的研究

用国产非离子型大孔网状树脂CAD—45吸附提取麦迪霉素，取代了传统的溶媒萃取法．试验确定了提取工艺条件：吸附最佳pH为8.3～8．5，流速为1／6ml／min；解吸前先用1％氨水1：1（V/V）洗柱；最佳解吸剂为醋酸丁酯，流速为1／12ml／min。收率可达84．8％。     

Preparative counter-current chromatography isolation of liensinine and its analogues from embryo of the seed of Nelumbo nucifera GAERTN. using upright coil planet centrifuge with four multilayer coils connected in series

Preparative counter-current chromatography (CCC) isolation of liensinine and its analogues, isoliensinine and neferine from embryo of the seed of Nelumbo nucifera GAERTN. has been successfully performed for the first time using upright coil planet centrifuge with four multilayer coils connected in series with 1600 mL capacity. Two kinds of two-phase solvent systems were applied to preparative CCC isolation. The first was the system composed of light petroleum (b.p. 60-90 degrees C)-ethyl acetate-tetrachloromethane-chloroform-methanol-water (1:1:4:4:6:2, v/v) which was very suitable for fast and small-scale CCC isolation. The second was the system composed of ethyl acetate-tetrachloromethane-methanol-water (1:6:4:1, v/v), which was the optimum for large-scale CCC isolation. Using the first system, 1102 mg of the crude alkaloid was purified in one-step separation of 150 min, yielding 350 mg neferine, 100 mg isoliensinine and 95 mg liensinine with over 95% purity. While using the second solvent system, 5850 mg of the crude alkaloid was purified in one-step separation of 9 h, yielding 2545 mg neferine, 698 mg isoliensinine and 650 mg liensinine with over 97% purity. Structures of the compounds were identified by electrospray ionization multiple mass spectrometry, one- and two-dimensional NMR.     

聚合离子液体-碳纳米管复合物在线固相萃取分离白蛋白

合成了聚（1-乙烯-3-乙基咪唑溴代盐）（poly（ViEtIm＋Br-））聚合离子液体,并通过π-π堆积将其固载到多壁碳纳米管上,得到了聚离子液体-碳纳米管复合物.以15mg复合物的填充柱为固相吸附剂,在顺序注射系统中研究了其对白蛋白的在线固相萃取分离纯化.在pH5.2时,对2mL溶液中（50μgmL-1）白蛋白的吸附效率为91%.0.04molL^-1柠檬酸盐缓冲溶液可定量洗脱吸附的白蛋白.整个分离纯化过程耗时500s,富集倍数为5.用该法对人全血中的白蛋白进行分离纯化,经SDS-PAGE凝胶电泳验证,得到了纯度较好的白蛋白.     

Infrared and thermal studies of uranyl(VI) complexes of antipyrine

Recently, the isolation and characterisation of a large number of uranyl(VI) complexes with neutral unidentate oxygen donor ligands having XO bonds (XC, N, P, S or As) have been reported [1–5]. Antipyrine (1-phenyl-2,3-dimethyl-5-pyrazolone), containing a polar carbonyl group, is found to form complexes with metal ions [6-13]. This communication describes the isolation and physico-chemical properties of the complexes formed by uranyl(VI) ions.     

New nonlinear optical polyurethanes with adjusted subtle structure through Sonogashira coupling reaction

In this paper, four new nonlinear optical (NLO) polyurethanes ( P1 – P4 ) were designed and synthesized, and according to the concept of “suitable isolation group,” the subtle structure of the obtained polymers were modified by the introduction of isolation groups in different sizes to adjust their properties via Sonogashira coupling reaction. All the polymers were well characterized and the second harmonic generation (SHG) experiment results demonstrated that BOP groups were the suitable isolation groups in this system, and the corresponding polymer P2 exhibited a larger d₃₃ value than other polymers. Thus, the obtained results further confirmed our original idea and were consistent with the concept of “suitable isolation group.” Copyright © 2009 John Wiley & Sons, Ltd.     

Anti-inflammatory diterpene from Thyrsanthera suborbicularis

Bioactivity-guided isolation on a n-hexane-soluble fraction of Thyrsanthera suborbicularis led to the isolation of a new rosane-type diterpene, 19-hydroxy-1(10), 15-rosadiene (1), along with three known compounds, taraxerol, acetyl aleuritolic acid, and spathulenol. The structures of isolated compounds were determined by interpretation of NMR spectroscopic data and mass spectrometry. Compound 1 demonstrated significantly inhibitory activity on nitric oxide production in RAW264.7 lipopolysaccharide (LPS)-activated mouse macrophages with an IC(50) value of 2.91 μg/ml via the suppression of inducible nitric oxide synthase (iNOS) mRNA expression.     

New sesquiterpene hydroperoxides with trypanocidal activity from Pogostemon cablin

Trypanocidal constituents of Pogostemon cablin were investigated. Activity guided isolation of the acetone extract resulted in isolation of three new sesquiterpene hydroperoxides 1-3, together with a known sesquiterpene, patchouli alcohol (4). In vitro minimum lethal concentrations of the hydroperoxides 1-3 against epimastigotes of Trypanosoma cruzi were 0.84 microM (1), 1.7 microM (2) and 1.7 microM (3). The activity of the corresponding alcohols and patchouli alcohol was very weak (MLC>200 microM).     

Two new diterpene alkaloids from Delphinium chrysotrichum

Chemical investigation on the ethanol extract from the whole plants of Delphinium chrysotrichum resulted in the isolation of two new diterpene alkaloids named delphatisine A (1) and delphatisine B (2), respectively. The structures of the new compounds were deduced on the basis of their spectral data (IR, HREIMS, EIMS, 1D, 2D-NMR). This is the first report on the isolation of diterpenoid alkaloids from the D. chrysotrichum.     

Antimicrobial, antileishmanial and cytotoxic compounds from Piper chaba

The petroleum ether and chloroform extracts of the root of Piper chaba showed antimicrobial, antileishmanial and cytotoxic activities. Further bioactivity-guided fractionation led to the isolation of Bornyl piperate (1), piperlonguminine (2) and piperine (3). This is the first report of isolation of compounds (1) and (2) from P. chaba. It was observed that the isolated compounds (1 and 2) showed potent antifungal activity when compared with standard drug Nystatin, and significant cytotoxic activity with the IC?? values of 0.76 and 0.83?μg?mL?1, respectively. These compounds were also found to have weak antibacterial and antileishmanial activities. This is the first report about the antileishmanial activity of Piper isolates.     

Selective dilithiation of [Ti(η(5)-C5H5)(η(8)-C8H8)] and subsequent conversion into neutral and cationic ansa-complexes

Selective dimetalation of a sandwich complex featuring the cyclooctatetraene ligand has been accomplished for the first time. The isolation of the dilithiated species 1 subsequently enabled the isolation of a paramagnetic [2]stannatitanoarenophane (2) via salt elimination reaction. Chemical oxidation resulted in the formation of a rare example of a cationic ansa-complex (3).     

4-Lithio-1-tritylimidazole as a synthetic intermediate. Synthesis of imidazole-4-carboxaldehyde

Reaction of 4-iodo-1-tritylimidazole with n-butyllithium at –79°, followed by rapid quenching of the reaction mixture with DMF, gives good yields of 1-tritylimidazole-4(5)-carboxaldehyde, the isolation of which demonstrates the intermediacy of 4-lithio-1-tritylimidazole. This species should be destabilized by repulsive interaction of the negative charge on C-4 with the adjacent lone pair electrons on N-3 (the ALP effect). The isolation of 1-tritylimidazole-4(5)-carboxaldehyde in good yield and the versatility of the aldehyde functionality make 4-lithio-1-tritylimidazole a useful synthetic intermediate.     

Optimized precursor ion selection for labile ions in a linear ion trap mass spectrometer and its impact on quantification using selected reaction monitoring

The fragmentation of fragile ions during the application of an isolation waveform for precursor ion selection and the resulting loss of isolated ion intensity is well‐known in ion trap mass spectrometry (ITMS). To obtain adequate ion intensity in the selected reaction monitoring (SRM) of fragile precursor ions, a wider ion isolation width is required. However, the increased isolation width significantly diminishes the selectivity of the channels chosen for SRM, which is a serious problem for samples with complex matrices. The sensitive and selective quantification of many lipid molecules, including ceramides from real biological samples, using a linear ion trap mass spectrometer is also hindered by the same problem because of the ease of water loss from protonated ceramide ions. In this study, a method for the reliable quantification of ceramides using SRM with near unity precursor ion isolation has been developed for ITMS by utilizing alternative precursor ions generated by in‐source dissociation. The selected precursor ions allow the isolation of ions with unit mass width and the selective analysis of ceramides using SRM with negligible loss of sensitivity. The quantification of C18:0‐, C24:0‐ and C24:1‐ceramides using the present method shows excellent linearity over the concentration ranges from 6 to 100, 25 to 1000 and 25 to 1000 nM, respectively. The limits of detection of C18:0‐, C24:0‐ and C24:1‐ceramides were 0.25, 0.25 and 5 fmol, respectively. The developed method was successfully applied to quantify ceramides in fetal bovine serum. Copyright © 2014 John Wiley & Sons, Ltd.     

A novel precipitating auxiliary approach to the purification of Baylis-Hillman adducts

Diaryl alkene alcohol 1 is a 'precipiton', a precipitating auxiliary that is used to aid the isolation of Baylis-Hillman adducts.     

Synthesis of a calix[4]arene derivative for isolation of a stable cation radical salt for use as a colorimetric sensor of nitric oxide

We have designed and synthesized a modified calixarene derivative (1) that allows, for the first time, the isolation of a stable cation radical salt that binds a single molecule of nitric oxide deep within its cavity with remarkable efficiency (KNO >108 M-1), as demonstrated by isolation of a crystalline complex [1, NO]+ and its characterization by X-ray crystallography as well as by optical spectroscopy. Furthermore, the ready accessibility of the calixarene cation radical will allow the exploration of its use for developing efficient sensing devices for nitric oxide based on the accompanied color changes.     

Tricalysionoside A, a megastigmane gentiobioside, sulfatricalysines A-F, and tricalysiosides X-Z, ent-kaurane glucosides, from the leaves of Tricalysia dubia

Further isolation work on the water-soluble fraction of a MeOH extract of Tricalysia dubia afforded one new megastigmane gentiobioside, named tricalysionoside A (1), and three sulfates, named sulfatricalysines A-C (2-4). Extensive isolation work on the 1-BuOH-soluble fraction of a MeOH extract of T. dubia yielded sulfatricalysines D-F (5-7) and three new ent-kaurane glucosides, named tricalysiosides X-Z (8-10). The structures of the new compounds were elucidated by analyses of one- and two-dimensional NMR spectroscopic data. The absolute stereochemistry of tricalysionoside A (1) was established by modified Mosher's method.     

New Spirostaphylotrichins from Staphylotrichum coccosporum

The isolation and structure elucidation of the new spirostaphylotrichins B ( 2 ), C and D ( 3/4 ), F ( 5 ), Q ( 6 ), and R ( 7 ) are described. Compounds 2 and 3 are artefacts formed during the isolation of the metabolites from the cultures. The absolute configuration of spirostaphylotrichin A ( 1 ) has been determined by CD spectroscopy.     

Eine neue,einfache Synthese von 2,3,5-Trichlorpyridin

A New Simple Synthesis of 2,3,5-Trichlorpyridine A simple synthesis of 2,3,5-trichloropyridine by the copper-catalyzed free radical addition of chloral to acrylonitrile with or without isolation of the primary 1:1 adduct,4-formyl-2,4,4-trichlorobutyronitrile ( 1 ), is described.