114 results about "Estrone" patented technology

The invention relates to a detecting technique of endocrine disrupters in water environment and particularly relates to a technique for quantitative analysis on oestrone, 17beta-estradiol, estriol, 17alpha-ethinyl estradiol, nonyl phenol, octylphenol and bisphenol A in a complex substrate water sample by adopting a liquid chromatogram-tandem mass spectrum combined technique. The method comprises the following steps: enriching a collected water sample by using a HLB (Hydrophile-Lipophile Balance) solid-phase extraction column and washing with carbinol; drying elution liquid nitrogen and purifying by using Florisil; and finally, analyzing by utilizing the liquid chromatogram-tandem mass spectrum combined technique. The method is environment-friendly, easy to operate and high in recovery rate. The method can quickly analyze the trace amount of oestrone, 17beta-estradiol, estriol, 17alpha-ethinyl estradiol, nonyl phenol, octylphenol and bisphenol A in the complex substrate water sample.

The invention discloses a derivatization method of environmental estrogens (estrone, 17beta-estradiol, estriol, 17alpha-ethynylestradiol), which is a treatment method and a core technology before a gas chromatography-mass spectrum (GC-MS) is used for analyzing the samples of the substances. The method comprises the following steps: firstly, leading high-purity nitrogen in at a room temperature to dry a standard mixed solution containing environmental estrogens; adding derivative reagents N, O-BSTFA and pyridine to react at room temperature (20 DEG C)-50 DEG C to obtain derivative products; drying; adding a sampling solvent and an internal standard; sampling and analyzing. The method has the advantages of simple and convenient experimental operation, time saving and low energy consumption and cost, simultaneously derivates the four environmental estrogens without generating side products, has favorable linear correlation among various derivative products and achieves an instrument detection limit up to 0.5pg/ muL, thereby being applied to the GC-MS detection of environmental estrogens in water bodies, sediment, biological samples, and the like.

The invention provides a method for performing gold-catalyzed selective C-H bond functionalization on phenol and aniline, which comprises the following steps: by taking phenol and aniline compounds as raw materials and taking phosphine ligand or carbene as ligand, in organic solvent, reacting with a diazo compound in the presence of a gold catalyst and a silver salt, performing carbon-hydrogen bond insertion at the para-position or ortho-position of the phenol or aniline structure. The method provided by the invention has the characteristics of low catalyst consumption, mild conditions, wide substrate application range and the like; the method can be used for quickly and efficiently synthesizing methyl acetate derivatives containing the phenol or aniline structure; and meanwhile, the method can be used for performing later modification on natural products or drug molecules (such as estrone), or be used for synthesizing some molecules having biological activity, thus having favorable application prospects.

Pseudomonas fluorescens capable of degrading estrogen substances is named as SJTE-2, and a preservation number is CGMCC No.6587. The pseudomonas fluorescens can use natural estrogen or environmental estrogen as the only carbon source to grow and can degrade estrogen substance oestrone, 17-Beta-estradiol, estriol and polycyclic aromatic hydrocarbon substance naphthalene, luxuriant, bisphenol A, and can be used for decomposing and removing an estrogen substance and a polycyclic aromatic hydrocarbon substance in an environment. Under the culture condition that the estrogen or the polycyclic aromatic hydrocarbon is used as the only carbon source, a bacterial strain SJTE-2 can degrade oestrone, 17-beta-estradiol and estriol within 24 hours, wherein the initial concentration of the oestrone, 17-beta-estradiol and estriol is 1 mg/L, and degradation rate of naphthalene, luxuriant and bisphenol A is over 90%, wherein the concentration of the naphthalene, luxuriant and bisphenol A is 50 mg/L. The bacterial strain can degrade oestrone, 17-beta-estradiol and estriol for more than 90% in 7 days, wherein the initial concentration of oestrone, 17-beta-estradiol and estriol is 50 mg/L, and degradation rate of naphthalene, luxuriant and bisphenol A is larger than 80%, wherein the concentration of naphthalene, luxuriant and bisphenol A is 500 mg/L.

The invention proposes a preparation method of estrone. The synthesis process route is shown in the formula (please see the formula in the specification). Leftovers ADD of soybean oil serve as raw materials to replace diene, the estrone is fast synthesized just through two steps of chemical reactions, energy consumption is reduced, pollution is reduced, and the three-waste yield of the method is only 1/10 of a traditional technology. Raw material sources are very wide, cost is low, and the preparation method is suitable for industrialized application and popularization. The obtained product is high in total yield. The purity is as high as 99.0% after processing is performed, the any individual impurity is smaller than 0.1%, and the estrone reaches the standard of the United States Pharmacopoeia. The mass yield is 60-65%.

The invention discloses a compound containing difluromethylation and a preparation method therefor. The invention provides a preparation method of a compound RCF2H containing the difluromethylation. The preparation method comprises the following steps of: under the protection of inert gas, performing a coupling reaction on a compound RX and trimethyl difluromethylation silicon in an organic solvent under the existing conditions of a palladium catalyst, a ligand and alkali so as to obtain the compound RCF2H containing the difluromethylation. Through the adoption of the difluromethylation reaction of the compound disclosed by the invention, the difluromethylation of the compound with various aryl halogen compounds such as aryl iodide, aryl bromide and natural products (such as estrone or vitamin E) can be realized, the conditions of the type of reactions are mild, raw materials are cheap and easy to obtain, the conversion rate of the reaction is high, the compatibility of base groups is good, and the compound has a good market application prospect. RX+TMSCF2H -> RCF2H

The present invention discloses a preparation method and uses of an anti-cancer drug estrogen targeting PEG-modified liposome. The liposome preparation method comprises: synthesizing estrone-pegylated phospholipid from activated estrone, taking 40-80 parts by weight of phospholipid, 5-45 parts by weight of cholesterol, and 5-40 parts by weight of pegylated phospholipid, dissolving in methanol, carrying out rotary evaporation, adding an ammonium sulfate aqueous solution, carrying out dialysis, adding 0.5-10 parts by weight of mitoxantrone, carrying out incubation, carrying out dialysis, adding 0.1-20 parts by weight of the estrone-pegylated phospholipid, carrying out incubation, and filtering with a membrane to obtain the liposome preparation. Compared with the liposome in the prior art, the obtained estrogen targeting PEG-modified liposome has characteristics of high encapsulation efficiency, uniform particle size, pharmacokinetics improving, anti-tumor efficacy enhancing, toxicity reducing, simple preparation process and easy scale-up production, and is expected to become the novel pharmaceutical preparation for cancer therapy. The uses are targeted treatments of breast cancer, leukemia and other cancers.

A process is provided for the making of estetrol starting from a 3-A-oxy-estra 1,3,5(10),15-tetraen-17-one, wherein A is a C₁-C₅ alkyl group, preferably a methyl group, or a C₇-C₁₂ benzylic group, preferably a benzyl group. This process is particularly suitable to industry.

The invention relates to a pseudomonas citronelloalis strain and application thereof in degrading estrogen, wherein the pseudomonas citronelloalis strain has the preservation number of CGMCC No.3634, can grow by using natural or synthetic estrogen as a unique carbon source, can efficiently degrade theelin (E1), 17beta-estradiol (E2) and 17alpha-ethinyl estradiol (EE2) and can be used for a micro-biological degradation technology for removing the estrogen. Under the culture condition of using the estrogen as the unique carbon source, the theelin and the 17beta-estradiol with the initial concentration of 2mg/L can be respectively degraded by 99 percent by the SS-2 strain within 36 hours, the 17alpha-ethinyl estradiol with the initial concentration of 4mg/L can be degraded by 93.6 percent within 168 hours, and estriol has no remarkable degradation phenomenon. The theelin is generated in the process of degrading the 17beta-estradiol, and the theelin is also gradually degraded. Because the pseudomonas citronellolis SS-2 strain has the characteristics of effectively degrading the natural and synthetic estrogen in an environment, the pseudomonas citronellolis SS-2 strain can be applied to an estrogen-contained waste sewage treatment technology or a soil remediation technology.

The present invention relates to the fields of analytical chemistry and food safety, and provides a method for simultaneously detecting residue quantities of multiple hormone veterinary drugs. The method comprises steps of: extracting a sample with acetonitrile; purifying by three SPE columns, including a C18 column, a silica gel column and an amino column; carrying out a microwave assisted derivatization reaction; and using a DB-5MS capillary column (0.25mm *30m *0.25 mum) to separate and detect residue quantities of nine hormone veterinary drugs. Detection limits of the method of the invention on the nine hormone veterinary drugs, including hexestrol, diethylstilbestrol, dienestrol, etiocholanolone, epitestosterone, oestrone, estradiol, ethinyloestradiol and estriol, are 0.1 mug / kg, 0.3 mug / kg, 0.15 mug / kg, 1mug / kg, 0.17 mug / kg, 0.3 mug / kg; 0.4 mug / kg, 0.35 mug / kg and 0.3 mug / kg respectively. The lower limit of detection of the method provided by the invention meets requirements of related domestic and foreign laws and regulations, and technical indicators, such as precision and recovery rate, are in line with the provisions of relevant standards.

The invention relates to an oat acidovorax avenae strain capable of biodegrading natural estrogen and the application thereof, and the preservation code is CGMCC No. 3633; natural estrogen serves as the only one carbon source and is grown, can degrade estrone, 17Beta-estradiol and estriol with high efficiency, and can be used for a microbial technology for removing estrogen. The SS-1 strain can degrade the estrone with the initial concentration of 1mg/L by 99 percent within 12h, and degrade the 17Beta-estradiol and estriol with the initial concentration of 1mg/L by 99 percent within 24h. Estrone is generated in the degradation process of 17Beta-estradiol, and the estrone is also gradually degraded. Because the acidovorax avenae SS-1 strain has the property of effectively degrading the natural estrogen in the environment, and thereby can be applied in a technology for controlling wastewater and sewage which contain estrogen or a soil restoration technology.

The invention discloses a method for preparing 19-demthyl-4-androstenedione, which comprises the steps of: based on estrone as a raw material, sequentially carrying out etherealization reaction, ketalation, Birch reducing reaction and hydrolysis reaction to obtain19-demethyl-4-androstenedione, wherein the reaction formula is shown in the specification. According to the method provided by the invention, the traditional phenolic group methyl etherealization process is improved, methyl carbonate replaces traditional high-toxicity carcinogenic etherealization reagents dimethyl sulfate and iodomethane, and inexpensive potassium carbonate is used as a base, so that the production cost is lowered, the method is environment-friendly, the yield is high, and the method is suitable for scaled industrial production.

The invention discloses a method for separating beta-estradiol and oestrone method based on a nanometer channel modified by an aptamer. A prepared array gold nanoparticle channel is used as a carrier and aptamer modifies beta-estradiol inside the gold nanoparticle channel so as to obtain a gold nanoparticle channel membrane which has special selectivity to the beta-estradiol. A difference of the beta-estradiol and the oestrone is utilized, transfer speed of the beta-estradiol and the oestrone in the nanometer channel which modifies the aptamer, the aptamer has the selectivity to the beta-estradiol, and comparatively passes through the modified nanometer channel, but the oestrone is not easy to pass through, and the separation of the beta-estradiol and the oestrone is achieved. The method can provide a novel idea for conducting compartment analysis to estrogens with different affinity of other aptamers.

The invention relates to 16alpha-methyl-3-hydroxyl-19-norpregnane-1, 3, 5-triene-20-ketone and a preparation method thereof. In the invention, degraded product of natural diosgenine petunidin 3-acetoxyl group-pregnane-5, 16-diene-20-ketone is used as the raw material, the raw material is methylated by aluminum methide before hydrolization, 1-dehydrogenation and A aromaticcyclizationofparaflins to prepare 16alpha-methyl estrone steroid compound 16alpha-methyl-3-hydroxyl-19-norpregnane-1, 3, 5-triene-20-ketone. The compound has activity suppression effect for breast cancer cellbeads MDA-MB-231, and the preparation method is characterized by easily available raw material and high yield.

The invention relates to the technical field of breeding of small yellow croakers, in particular to a feminization inducing method for small yellow croakers with undifferentiated sex glands. The method comprises the following steps: placing fry of small yellow croakers hatched for 13-15 days and having undifferentiated sex glands in seawater containing estrogen with a low concentration of 1-10 [mu]g/L for dipping bath, and performing dipping bath for 2 hours every day and continuous for 60 days, so as to enable the crowd of small yellow croakers to be completely feminized, wherein the selectable estrogen comprises estrone, soybean isoflavone, estradiol, estriol, coumestrol and genistein. The effect of estradiol is more obvious, 1 [mu]g/L estradiol can ferminize 96.6% of a crowd of small yellow croakers, 10 [mu]g/L estradiol can ferminize 100% of a crowd of small yellow croakers, the induction rate is high, the operatability is high, natural environment does not cause limit. Female parent fish guarantee is provided for large-scale artificial breeding of small yellow croakers, a technological route is opened up for study on sex control and monosex breeding of small yellow croakers, and a route for solving the problem of less of female population of small yellow croakers is provided.

The invention discloses a novel byproduct produced by an ethinyloestradiol synthesis process and a synthesis method thereof. The byproduct is as shown in a formula I, and the chemical name is 3-hydroxy-19-nor-17alpha-pregna-1,3,5(10)-triene-20-(3-hydroxy-3-methylbutynyl-1-yl)-17-ol. The invention also provides a preparation method of the byproduct. The substance can be simply and conveniently obtained by performing Grignard exchange on alkyl magnesium bromide and 3-methyl-1-butynyl-3-ol and then performing Grignard exchange on estrone. The compound can be used as a standard substance for controlling impurities in an ethinyloestradiol production process.

The invention discloses an in-situ fixative for estrone-contaminated soil, and a preparation method and an application thereof. The above repairing material is nanometer iron-manganese modified litchibiochar prepared by high-temperature anaerobic rapid pyrolysis. The preparation method of the nanometer iron-manganese modified litchi biochar comprises the following steps: mixing the prepared litchi biochar with a 0.1 mol/L potassium permanganate solution and a 0.1 mol/L ferric chloride solution, carrying out an ultrasonic reaction at 40 DEG C for 2 h, oscillating the obtained solution at normal temperature for 2 h, and carrying out high-temperature anaerobic rapid pyrolysis to the obtain the nanometer iron-manganese modified litchi biochar. When the estrone-contaminated soil is doped withthe nanometer iron-manganese modified litchi biochar, estrone is not detected in a leachate within 96 h. The nanometer iron-manganese modified litchi biochar can realize the reuse of solid wastes in the forestry and fruit industry, and effectively control the migration of estrone in soil contaminated due to livestock and poultry breeding and significantly reduce the risk of estrone contamination.

The invention discloses a preparation method of modified pollen and the application thereof for absorbing and treating EDCs of water, which belong to a treatment method for sewage or wastewater. The preparation method disclosed by the invention comprises the following steps: washing natural pollen with ethanol; carrying out solid-liquid separation, drying and crushing; and adding the crushed product into a concentrated hydrochloric acid, sequentially carrying out ultrasonic dispersion and backflow filtering, washing to neutral, and drying, wherein the natural pollen is lotus pollen, piny flower pollen, apricot flower pollen and dandelion pollen. According to the application of the modified pollen for treating EDCs of waer, the modified pollen is added into water containing pollutants such as bisphenol A, estrone, 17beta-estradiol, estriol, progesterone, 17-alpha-ethinyl estradiol, 4-n-nonyl phenol, 4-t-octyl phenol, diethylstilbestrol or tetrabromobisphenol A. The pollen disclosed by the invention is small in polarity, hydrophobic, high in adsorbent active site and saturated adsorption amount, small in desorption ratio, renewable and reusable, therefore, the application is a way of treating water pollutions by using biomass materials.

A pseudomonas putida strain capable of efficiently degrading estrogen is named as SJTE-1. Preservation number of the pseudomonas putida strain is CGMCC No. 6585. The pseudomonas putida strain can grow by using natural or synthesizing estrogen as only carbon source, can efficiently degrade estrone (E1), 17-beta estradiol (E2), estriol (E3) and 17-alpha ethinyl estradiol (EE2), and can be used for modifying environments polluted by estrogen. Under the condition that the estrogen is used as the only carbon source, the SJTE-1 can degrade 99% of estrone, 17-beta estradiol, and estriol 1mg/L in initial concentration in 24 hours, can degrade more than 95% of estrone, 17-beta estradiol, and estriol 50mg/L in initial concentration in 168 hours, and degrading rate of 17-alpha ethinyl estradiol 5mg/L in initial concentration is more than 90%. Estrone generated during degrading of 17-beta estradiol is also degraded into estrogen-free active substances.

Syntheses of steroids such as 3-hydroxy-7α-methyl-21-[2′-methoxy-4′-(diethylaminomethyl)-phenoxy]-19-norpregna-1,3,5(10)triene citrate (“SR 16234”) and analogs thereof are provided, wherein 21-hydroxy-19-norpregna-4-en-3-one serves as a starting material or intermediate. The latter compound may be readily prepared from estrone-3-methyl ether. Certain intermediates in these syntheses also have value as therapeutic agents, for example in the treatment of prostate disorders such as prostatic cancer.

Compounds, pharmaceuticals, cosmetic or dietary supplements for the treatment of overweight, obesity and/or type II diabetes in a mammal (e.g. human) comprising a compound with formula I or formula II for example ceramidase-inhibitor, such as (1S,2R)-D-erythro-2-(N-myristoylamino)-1- phenyl-1-propanol, alone or in combination with an anorexic lipid (or other appetite-inhibiting acylamides or oleoyl-estrone), and methods of treatment comprising administration of said compounds, pharmaceuticals, cosmetic or a dietary supplements. The compounds, pharmaceuticals, cosmetic or dietary supplements and methods of the invention may further be used in modifying the feeding behaviour, suppression of hunger, enhancement of satiety, reduction of energy intake, reduction of fat tissue mass/lean mass ratio in a mammal (e.g. human).

The invention discloses a panda oestrone peak time prediction method and application thereof. The panda oestrone peak time prediction method comprises the steps of: when a female panda enters an oestrus season and the vulva color becomes red, collecting panda urine, and measuring the content of creatinine, oestrone and progesterone in the panda urine respectively; when the creatinine content is greater than 0.2 mg/mL, calculating the oestrone content after creatinine correction; when the oestrone content after creatinine correction is greater than 20 ng/mg Cr for the first time, indicating panda oestrus starting, recording a panda urine collection time point as oestrus starting time, extending backwards for 4 days from the starting time, performing E/P value calculation on panda urine of which the creatinine content is greater than 0.2 mg/mL and the progesterone content is greater than 2.5 ng/mL, and determining a target E/P value according to the E/P value; and determining appearancetime of a panda oestrone peak value according to the panda urine collection time point corresponding to the target E/P value. The panda oestrone peak time prediction method is high in prediction timeperiod accuracy degree, good in repeatability, simple to operate and small in workload.

The invention relates to an oestrone derivative for detecting oestrone content in a biological sample and a preparation method of the oestrone derivative. The structural formula of the oestrone derivative is shown as a formula (I). Oestrone immunogens with high immunogenicity and corresponding antibodies are prepared in succession by using the oestrone derivative. The oestrone immunogen is high inspecificity and high in immunogenicity, and the anti-oestrone specific antibody is high in specificity and high in titer, is capable of well recognizing and binding oestrone, and does not have any cross reaction with common 92 chaff interferents. The invention further discloses an oestrone enzyme-labeled conjugate, and an oestrone homogeneous enzyme immunoassay detection reagent is prepared by utilizing the anti-oestrone specific antibody and the oestrone enzyme-labeled conjugate. The reagent is capable of conveniently, rapidly, and accurately measuring the oestrone content in the biologicalsample, multiple samples are determined on a full-automatic biochemical analyzer, high throughput and rapid determination of the oestrone is realized, the accuracy is high, the specificity is high, and the accuracy and detection efficiency are greatly improved compared with the previous detection.

A compound of formula (I)

(where X₁ and X₂ represent independently a hydrogen atom or a group of formula (II)

R₁ represents a linear or branched halogenoalkyl group having 1-7 carbon atoms; Ra represents a hydroxyl group and Rb represents a linear or branched alkynyl group having 2-5 carbon atoms, or Ra and Rb, when taken together with the carbon to which they are bound, represent a carbonyl group; m is an integer of 2-14; n is an integer of 2-7; provided that X₁ and X₂ are not both a hydrogen atom), stereoisomers of the compound, or hydrates, salts or esters thereof, as well as a pharmaceutical composition containing a therapeutically effective amount of the compound.