新法合成Cu_2(Benzoate)_4(Caffeine)_4及其性质

新法合成了铜()、咖啡因、苯甲酸的三元配合物,并用红外光谱、元素分析、X-单晶衍射和热重分析进行了表征,配合物与ct-DNA作用的紫外-可见吸收光谱表明配合物能以嵌入的方式与ct-DNA作用,结合常数Kb=1.5×104mol/L。

Hydrothermal Synthesis and Thermal Decomposition Mechanism of Alkaline Earth Benzoates

Alkaline earth benzoates were synthesized using hydrothermal reaction. The complexes were characterized by elemental analysis, IR, X ray powder diffraction. All of them are monoclinic and have layered structure. The mechanism of thermal decomposition of alkaline earth benzoates was studied by using TG, DTA, IR and gas chromatography mass spectrometry. The thermal decomposition of alkaline earth benzoates in nitrogen proceeded in one or two stages: they decomposed to form MCO 3 (M=Ca,Sr,Ba) or MgO and organic compounds, respectively. The organic compounds obtained from decomposition reaction are mainly benzophenone, triphenylmethane and so on.

Rizatriptan benzoate influences the endogenous pain modulatory system in a rat model of migraine

The present study utilized a nitroglycerin-induced rat model of migraine to detect the effects of rizatriptan benzoate on proenkephalin and substance P gene expression in the midbrain using real-time quantitative polymerase chain reaction and investigate whether rizatriptan benzoate can regulate the endogenous pain modulatory system. The results showed that rizatriptan benzoate significantly reduced expression of the mRNAs for proenkephalin and substance P. Rizatriptan benzoate may inhibit the analgesic effect of the endogenous pain modulatory system.

STUDY ON THE THERMODYNAMIC PROPERTIES OF ADSORPTION OF ETHYL BENZOATE AND DIETHYL PHTHALATE BY PHENOLIC RESIN ADSORBENTS

This paper presents experimental observations on the adsorption of individual solutes by a simple thermodynamic framework, and the equilibrium adsorption of ethyl benzoate and diethyl phthalate on phenolic resin adsorbent in hexane solutions within the temperature range of 293-313 K. The experimental results show that the Freundlich adsorption law is applicable to the adsorption of ethyl benzoate and diethyl phthalate on the adsorbent, since all the correlative factors R' are larger than 0.99. The negative values of all the isosteric adsorption enthalpies for ethyl benzoate and diethyl phthalate indicate that they undergo exothermic processes, while their magnitudes (19-28 kJ/mol) manifest a hydrogen bonding sorption process. Other thermodynamic properties: the free energy changes and the entropy change associated with the adsorption have been calculated from the Gibbs adsorption equation and the Gibbs-Helmholtz equation

Synthesis, Crystal Structure and Antitumor Activity in Vitro of a New Benzoate Binuclear Cupper(Ⅱ ) Complex

The title compound, [Cu2（C7H5O2）4（C2H6O）2], was synthesized by the reaction of benzoic acid, copper acetate and ethanol in an aqueous solution. Trypan blue dye exclusion method was used in experiment. X-ray single-crystal analysis has revealed that compound 1 （C32H32Cu2O10） crystallizes in the monoclinic system, space group C2/c, Mr = 703.66, a = 47.340（5）, b = 6.6613（4）, c = 22.028（2）A,β = 113.284（4）°, V = 6380.6（10） A^3, Z = 8, Dc= 1.465 g/cm^3, F（000） = 2896,μ = 1.388 mm^-11, the final R = 0.0515 and wR = 0.1172 for 5712 observed reflections with I 〉 2σ（I）. X-ray crystal structure analysis suggests that compound [CH2（C7H5O2）4（C2H6O）2] has a binuclear structure with two Cu（II） atoms coordinated by four benzoate groups and two ethanol molecules. The crystal packing is stabilized by intermolecular O-H...O hydrogen bonds. The compound inhibits the proliferation of K562 cells （chronic myeloid leukemic cells） significantly and dose-dependently in 48 h, and IC50 of K562 is 17.3μg/mL by trypan blue dye exclusion method.

Release performance and sustained-release efficacy of emamectin benzoate-loaded polylactic acid microspheres

High-performance liquid chromatography （HPLC） was employed to determine drug release rates based on emamectin benzoate concentrations in the medium. Release kinetics equations were used to fit the drug release behavior. The effects of particle size and release medium pH on the release rate were also investigated. The indoor toxicity of emamectin benzoate-loaded polylactic acid microspheres on the diamondback moth larva （Plutella xylostella） was studied to explore drug sustained-release performance. In acidic and neutral media, the drug release behavior of the microspheres was in accord with the first-order kinetics equation. Increasing the spray dosage of emamectin benzoate-loaded polylactic acid microspheres initially resulted in an equivalent insecticidal efficacy with the conventional emamectin benzoate microemulsion. However, the drug persistence period was four-fold longer than that observed using the conventional formulation. The developed emamectin benzoate-loaded polylactic acid microspheres showed dramatic sustained-release performance. A treatment threshold of greater than 35 mg mL-1 was established for an efficient accumulated release concentration of emamectin benzoate-loaded microspheres.

Emamectin benzoate 9.7%SL as a new formulation for a trunkinjections against pine wood nematode,Bursaphelenchus xylophilus

In this study,we investigated the preventive effects of emamectin benzoate 9.7%SL,which was newly developed to reduce the injection volume and number of injection holes required to protect against pine wood nematode.None of the Pinus thunbergii trees injected with emamectin benzoate 9.7%SL at 0.3 mL/cm diameter at breast height(DBH)died within 2 years of inoculation with pine wood nematodes.Emamectin benzoate 9.7%SL injected at 0.6 mL/cm DBH resulted in no tree mortality for 3 years.Mean residue of emamectin benzoate 9.7%SL in pine twigs injected with 0.3 mL/cm DBH was 0.490μg/g at 1 year after injection and 0.303μg/g after 2 years.These residues values are greater than 0.031μg/g,previously determined IC95 value for emamectin benzoate against the pine wood nematode.Our field experiment and residue analysis showed that emamectin benzoate 9.7%SL could be a substitute agent for emamectin benzoate 2.15%EC,which is widely used to prevent pine wood nematode in the field and that injection volume and number of injection holes can be greatly educed using this new formulation,which will reduce injury to the cambium,interruption of water movement,and infection of inoculation wounds by wood-decay or blue stain fungi.

A developed HPLC method for the determination of Alogliptin Benzoate and its potential impurities in bulk drug and tablets

Alogliptin(AGLT),active ingredient of Alogliptin Benzoate(AGLT-BZ),is a new dipeptidyl peptidase-4(DPP-4)inhibitor for the treatment of type 2 diabetes.This study aimed to build a suitable method to determine the potential related substances in AGLT-BZ bulk drug and tablets.Seven related substances in Alogliptin Benzoate substances were synthetized and identified by ^(1)H-NMR and ESI-MS.In addition,the impurities were detected by a gradient reverse-phase high performance liquid chromatography(RP-HPLC)with UV detection.The chromatographic system consisted of an Angilent Zobax SB-CN column(250×4.6 mm;5 μm).The mobile phase consisted of water/acetonitrile/trifluoroacetic acid 1900:100:1 v/v/v(solution A)and acetonitrile/water/trifluoroacetic acid 1900:100:1 v/v/v(solution B)using a gradient program at a flow rate of 1.0 ml/min with 278 nm detection and an injection volume of 20 ml.Additionally,selectivity,the limit of quantitation(LOQ)and limit of detection(LOD),linearity,accuracy,precision and robustness were determined.Linearity was good over the concentration range 50-1000 ng/ml and the coefficient of determination(R^(2))were 0.9991-0.9998.RSD% of the determination of precision were <2%(n=6).The method of RP-HPLC for the determination of impurities in AGLT-BZ was proved to be precise,accurate,robust and reliable.Three batches of self-made bulk drug and three dosages of commercial tablets were detected with this method.

Effects of sodium benzoate on growth and physiological characteristics of wheat seedlings under compound heavy metal stress

In this study, we investigated the effect of exogenous sodium benzoate on wheat seedlings(Yangmai 16) grown under heavy metal stress. The results showed that 2.4 mmol kg-1 of heavy metals significantly inhibited growth and delayed emergence of wheat seedlings. Under compound heavy metal stress, application of 2-4 g L^-1 sodium benzoate significantly increased(P<0.01) chlorophyll content and chlorophyll fluorescence parameters Fv/Fm and Fv/Fo of wheat, compared to the control(water treatment). Further analysis showed that application of 2-4 g L^-1 sodium benzoate alleviated osmotic stress by promoting the accumulation of osmolytes such as soluble proteins and free proline, increased the activity of superoxide dismutase(SOD) and reduced malondialdehyde content(MDA). In contrast, higher concentrations of sodium benzoate solution(>6 g L^-1) inhibited the growth of wheat seedlings and even caused damage to seedlings. Correlation analysis showed that when the sodium benzoate concentration was in the range of 1.97-3.12 g L^-1(2016) and 1.58-3.27 g L^-1(2017), values of chlorophyll and its components, root activity, SOD activity, soluble protein, and free proline content were the highest. When the sodium benzoate concentration was raised to 2.59 g L^-1(2016) or 3.02 g L^-1(2017), MDA content was the lowest. Ultimately, exogenous sodium benzoate(2-4 g L^-1) facilitates root development and improves the root activity of wheat seedlings grown under compound heavy metals stress, thereby effectively alleviating the damage of compound heavy metal stress in wheat seedlings.

Synthesis, Bioactivity, and Crystal Structure Analysis of 2-(3-Oxobenzo[d]isothiazol-2(3H)-yl)ethyl Benzoates

Fifteen novel 2-（3-oxobenzo[d]isothiazol-2（3H）-yl）ethyl benzoates were synthesi- zed by the condensation of 2-（2-hydroxyethyl）benzo[d]isothiazol-3（2H）-one with substituted benzoic acids in dichloromethane. All the compounds were characterized by elemental analysis, IR, ESI-MS and 1H NMR. The crystal structures for 2-（2-hydroxyethyl）benzo[d]isothiazol-3（2H）-one （2） and 2-（3-oxobenzo[d]isothiazol-2（3H）-yl）ethyl 2-methoxybenzoate （30） have been determined by X-ray crystal structure analysis. Compound 2 （C9H9NO2S） crystallizes in the monoclinic system, space group Pn with a = 10.552（3）, b = 7.849（2）, c = 10.765（4） A, β = 103.128（4）°, V= 868.3（5） A3, Mr = 195.24, Dc = 1.493 Mg.m-3, μ = 0.33 mm-1, F（000） = 408, Z = 4, R= 0.0314 and wR= 0.0628. Compound 30 （C17H15NO4S） crystallizes in the triclinic system, space group P1 with a = 8.028（2）, b = 9.300（2）, c = 10.430（3）A, V= 752.1（3）A3, Mr = 329.36, D,= 1.454 Mg.m-3, p = 0.24 mm-1, F（000） = 344, Z = 2, R = 0.0377 and wR = 0.0904. The preliminary biological test indicated that the title compounds show better growth inhibitory activity against the gram-positive bacteria than the gram-negative bacteria.

Synergistic Activity of Organosilicone to Emamectin Benzoate against Beet Armyworm (Spodoptera exigua Hübner)

Based on determination for surface tension of organosilicone solution and its expansion on the solid surface, the biological activity of 5% emameetin ben- zoate WDG with organosilicone against beet armyworm was determined by spraying method to study their synergistic activity. The results showed that organosilicone significandy reduced surface tension of aqueous solution, and the surface tension was reduced to 26raN/m as the concentration of organosilicone was 0.01%. The organosilicone significantly raised expansion of liquid drops on solid surface, and the expansion diameter of 10 μL 0.01% organosilicone was 34 ram. The indoor toxicity results indicated that when addition dosage of organosilieone was 1% -5%, synergistic activity of 5% emamectin benzoate WDG with organosilicone against beet armyworm was significant, and increase extent of synergistic activity slowed down as organosilieone dosage was higher than 5%. Field experiment showed that the control efficacies of 5% emamectin benzoate WDG ＋5% organosilicone 33 mg/ L against beet armyworm were 81.57% and 82.66% after spraying for 3 and 7 d respectively, which were significandy better than treatments of 5% emamectin benzoate WDG 33 rag/L, 24% metaflumizone SC 96 mg/L, 5% chlorantranilip- role SC 33 mg/L, 20% tlubendiamide WDG 40 mg/L and 15% indoxacarb EC 43 mg/L.

A Novel RP-HPLC Method for Estimating Fulvestrant, Benzoyl Alcohol, and Benzyl Benzoate in Injection Formulation

For the quantitative determination of Fulvestrant, Benzyl alcohol, and Benzyl benzoate in Fulvestrant injection, an original RP-HPLC approach was developed. The gradient method was developed using HPLC and a Phenomenex Luna C8, 150 × 4.6 mm, i.d 3.0 μm particle size column with a gradient programme of mobile phases A and B. With a flow rate of 1.5 mL/minute, injection volume of 10 μL, and column temperature of 35°C, UV wavelength detection at 254 nm for Benzyl alcohol and Benzoyl Benzoate and 280 nm for Fulvestrant, mobile phase-A consists of DI water and mobile phase-B consists of Acetonitrile. The current study describes a single HPLC method for developing a Fulvestrant (Active), Benzyl alcohol (Cosolvent), and Benzyl Benzoate (Cosolvent) assay for Fulvestrant injection. The assay method was determined to be suitable for quantifying three components in the pharmaceutical product and was verified according to ICH guidelines.

Development and Validation of UV Spectrophotometric Method to Study Stress Degradation Behaviour of Rizatriptan Benzoate

Rizatriptan benzoate is a 5HT 1B/1Dreceptor agonist which is prescribed for the treatment of migraine.In the present study new,simple,specific ultraviolet spectrophotometric method for rizatriptan benzoate was developed and validated.Forced degradation studies were carried out in acidic,alkaline and neutral pH conditions.The absorbance maxima peak was found to be 224 nm and linearity was observed in the concentration range of 0.5~2.5μg·mL-1 with regression coefficient value of 0.998 8.The method was validated and found to be precise.The percent recovery for rizatriptan benzoate was found to be 98.576±0.202.The bulk drug was found to be stable in neutral and acidic pH conditions but got degraded in 1N NaOH solution.

Synthesis and Thermal Decomposition Mechanism of Rare Earth Benzoates

The rare earth metal benzoates were synthesized using hydrothermal reaction. The complexes were characterized by elemental analysis, IR and X-ray powder diffraction. They can be represented by general formula RE (C6H5COO)(3)(RE = La, Nd, Sm, Eu, Gd, Dy and Er). All of them are monoclinic and have layered structure. The mechanism of thermal decomposition of rare earth metal benzoates was studied by using TG, DTA, IR, and gas chromatography-mass spectrometry. The thermal decomposition of the rare earth benzoates in nitrogen proceeded in two stages; firstly it decomposed to form RE2O(CO3)(2) and organic compounds, then RE2O(CO3)(2) decomposed further to form rare earth metal oxides and carbon dioxide. The organic compounds obtained from the first step of the reaction are mainly benzophenone, 9,10-anthraquinone, 1, 3-Diphenylisobenzofuran and so on.

Synthesis and Crystal Structure of Tetranuclear Zinc Benzoate

A tetranuclear zinc benzoate Zn4O(C6H5CO2)6 was synthesized and characterized by X-ray single crystal determination. It crystallizes in cubic, space groupIa-3d. Its crystal cell is very large,a=4. 100 63 (18) nm, V=68.953(5) nm3 and Z=48. The structure is composed of discrete Zn4O(C6H5CO2)6 molecules. In each molecule, four zinc atoms are held together by a central oxygen atom, which results in the formation of a regular tetrahedron. All benzoate ligands coordinate to zinc atoms in a bidentate bridging mode. Each zinc atom is in a slightly distorted tetrahedral geometry, coordinated by three benzoate oxygen atoms and the central oxygen atom. The intermolecular interactions result in the formation of a three-dimensional supramolecular framework, with non-intersecting parallel channels. Key words tetranuclear - zinc benzoate - crystal structure - intermolecular interactions - channels CLC number O 623.621 Foundation item: Supported by the National Natural Science Foundation of China (20471044)Biography: YIN Ming-cai (1973-), female, Ph. D, research direction: functional coordination compounds.

Synthesis, Crystal Structure and Thermal Stability of a Saturated Dimeric Ce(III)-chelated Complex Based on Benzoate and 1,10-Phenanthroline Ligands

The title complex, [Ce（BA）3phen]2 （BA = benzoate, phen = 1,10-phenanthroline）, was prepared by the reaction of Ce（NO3）3.6H2O, benzoic acid and 1,10-phenanthroline. The complex was characterized by single-crystal X-ray diffraction, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is of triclinic, space group P1 with a = 10.912（2）, b = 11.962（3）, c = 12.474（3） A, α = 104.889（3）, β = 93.523（3）, γ = 113.332（3）^o, C66H46Ce2N4O12, Mr = 1366.90, V= 1420.2（6） ,A^3, Z = 1, Dc = 1.598 g/cm^3, μ = 1.652 mm^-1, S = 1.024 and F（000） = 682. The final R = 0.0391 and wR = 0.0947 for 4878 observed reflections with I 〉 2σ（I）. The structure of the title complex consists of two Ce（C6HsCOO）3（C12H8N2） units, forming a binuclear molecule. Each Ce（Ⅲ） is coordinated by two O atoms of one bidentate chelating carboxylate group, five O atoms of two bidentate bridging and two tridentate chelating-bridging carboxylate groups, and two N atoms of one 1,10-phenanthroline molecule to complete a distorted monocapped square antiprism geometry. Its thermogravimetric analysis was determined by TG-DTG techniques.

Residue and Safety Use of Emamectin Benzoate in Ginger

[Objective]The paper was to guide scientific and rational use of emamectin benzoate in ginger.[Method]A field experiment was conducted to determine residue and degradation dynamics and final residue of emamectin benzoate in ginger.The residue of emamectin benzoate in ginger was determined by high performance liquid chromatography-mass spectrometry(HPLC-MS/MS).[Result]The half-life of emamectin benzoate in ginger was 2.2-3.4 d.As 5%emamectin benzoate WDG was sprayed on ginger at 7.5 and 11.25 g·a.i/hm^2 for consecutive 1-2 times,the residues of emamectin benzoate in ginger harvested at 7,14 and 21 d post spraying were lower than the quantitative limit of the method(0.01 mg/kg),and were lower than the stipulation in Japan as well(0.1 mg/kg).[Conclusion]It is safe to use emamectin benzoate in ginger with the harvest interval of 7 d according to the recommended dose.

SPECTROSCOPIC STUDY AND APPLICATION ON THE INCLUSION COMPLEXATION β-CYCLODEXTRIN WITH ESTRADIOL BENZOATE IN AQUEOUS SOLUTION

The inclusion complexation reaction of β-cyclodextrin with estradiol benzoate (EB) in the presence ofcetyltrimethylammonium bromide has been studied by means of UV absorption and fluorescent spectrometry. The reaction conditions, the formation constant, the mechanism of the host-guest inclusion complexhave been studied and a simple, highly sensitive fluorescent synergistic method for the determination of EBhas been established with satisfactory results.

Activated Carbon and Clay Minerals for the Sorptive Removal of Denatonium Ions from Denatonium Benzoate Solutions

This study assessed the feasibility of utilizing activated carbon and clay minerals for treating water impacted with the bittering agent denatonium benzoate (DB). Our specific study objectives were to 1) evaluate denatonium ion sorption to smectite clay minerals (bentonite and hectorite) and activated carbon (powdered and granular) at constant pH and ionic strength and 2) examine the impact of pH on denatonium ion sorption to each solid material. The experimental results indicated that high doses (33,000 mg/L) of as-received granular activated carbon and as-received clay minerals completely removed denatonium from aqueous solutions containing 100 - 1000 mg/L denatonium benzoate. Powdered activated carbon at doses of 5 - 100 mg/L exhibited favorable monolayer sorption of denatonium ions from a pH 6.95, 70 mg/L aqueous denatonium benzoate solution with a Langmuir separation factor (r) of 0.481, a maximum sorption capacity (Sm) of 74 mg/g, and a Langmuir constant of 15.3 L/g. A maximum removal of 23% of denatonium was achieved at the highest powdered activated carbon dosage employed. Denatonium ion removal with peroxide treated bentonite and peroxide treated hectorite did not result in complete removal of the ion and exhibited favorable sorption as evidenced by Freundlich 1/n values ranging from 0.803 to 1.194;Freundlich constants (Kf) ranged from 8 ng/L to 575 ng/L. Denatonium ion sorption to peroxide treated bentonite appeared to depend on pH while hectorite sorption of denatonium ions was independent of hydrogen ion concentrations. For powdered activated carbon adsorption, as pH increased denatonium ion sorption decreased. Overall, the work demonstrates that denatonium can be effectively removed from water via activated carbon or clay mineral sorption.

RUTHENIUM CARBENE INITIATED RING-OPEN METATHESIS POLYMERIZATION OF ENDO-BICYCLO[3.2.0]HEPT-6-EN-3-YL BENZOATES WITH TACTICITY STUDIES

After tentative ring-opening cross metathesis （ROCM） of endo-bicyclo[3.2.0]hept-6-en-3-yl 4-bromobenzoate with PhCH = CH2 initiated by （Cy3P）2Cl2Ru = CHPh in CH2Cl2, ring-opening metathesis polymerization （ROMP） of a series of endo-bicyclo[3.2.0]hept-6-en-3-yl benzoates was achieved under the same conditions, furnishing a variety of the corresponding polymers. Then some of them were selected to hydrogenate the C=C double bonds in their backbone with p-tosylhydrazide, affording saturated and thus more flexible polymers. All of these polymers were well characterized by spectroscopic means including GPC, UV-Vis, NMR and IR, based on which the tacticity of these polymers was investigated together with nonlinear optical （electric-field-induced second-harmonic generation, EFISH）） analysis.