摘要：【中文】本发明属于多肽药物制备方法技术领域，特别涉及一种制备利拉鲁肽的方法。包括以下步骤：通过Fmoc固相合成法将Fmoc‑Glu‑2‑R侧链羧酸连接到氨基类型树脂A上得Fmoc‑Glu(Resin)‑R氨基酸树脂I；再通过多步骤固相偶联反应合成利拉鲁肽肽树酯，最后在酸性条件下裂解、色谱纯化、冷冻干燥得到高纯度利拉鲁肽。本发明解决了利拉鲁肽序列中Gln难耦合的难题，且将Glu侧链连接到氨基树脂上，Glu侧链相对较长，增加了肽链与树脂之间的柔性，使肽链更容易变形而降低反应位阻，该方法不需要使用钯催化体系，避免了钯金属的引入，从而提高合成反应效率和利拉鲁肽产品质量。 【EN】The invention belongs to the technical field of preparation methods of polypeptide medicaments, and particularly relates to a method for preparing liraglutide. The method comprises the following steps: connecting Fmoc-Glu-2-R side chain carboxylic acid to amino resin A by Fmoc solid phase synthesis to obtain Fmoc-Glu (resin) -R amino acid resin I; and synthesizing the liraglutide peptide resin through multi-step solid-phase coupling reaction, and finally cracking, chromatographic purification and freeze drying under an acidic condition to obtain the high-purity liraglutide. The invention solves the problem that Gln in a liraglutide sequence is difficult to couple, and the Glu side chain is connected to the amino resin, and is relatively longer, so that the flexibility between the peptide chain and the resin is increased, the peptide chain is easier to deform, and the reaction steric hindrance is reduced.

摘要：【中文】本发明属于医药技术领域，具体提供了一种西司他丁钠中间体的制备方法。包括以下步骤：以7‑X‑2‑氧代庚酸乙酯与(s)‑2，2‑二甲基环丙烷甲酰胺为原料，依次在催化剂、浓盐酸和氯化氢气体的作用下，经过：“一锅煮”方法简便地制得(Z)‑7‑X‑2((2s)‑2，2‑二甲基环丙烷甲酰胺基)‑2‑庚烯酸粗品，再经过重结晶得到(Z)‑7‑X‑2((2s)‑2，2‑二甲基环丙烷甲酰胺基)‑2‑庚烯酸精制品。本发明合成路线简短、操作简单、所得产品纯度较高，适合工业化生产。 【EN】The invention belongs to the technical field of medicines, and particularly provides a preparation method of a cilastatin sodium intermediate. The method comprises the following steps: taking 7-X-2-oxoheptanoic acid ethyl ester and(s) -2, 2-dimethylcyclopropanecarboxamide as raw materials, and sequentially carrying out the following steps under the action of a catalyst, concentrated hydrochloric acid and hydrogen chloride gas: the method of 'one-pot boiling' is simple and convenient to prepare a crude product of (Z) -7-X-2((2s) -2, 2-dimethylcyclopropane formamido) -2-heptenoic acid, and a refined product of (Z) -7-X-2((2s) -2, 2-dimethylcyclopropane formamido) -2-heptenoic acid is obtained by recrystallization. The method has the advantages of short synthetic route, simple operation and higher purity of the obtained product, and is suitable for industrial production.

摘要：【中文】本发明属于医药技术领域，具体公开了一种乌拉立肽杂质，通过样品跟踪监测，发现乌拉立肽甲硫氨酸氧化物贯穿整个乌拉立肽纯化工艺，并在乌拉立肽纯化后期，成为主要杂质成分。本发明还公开了该杂质的制备方法和检测方法，本发明制备方法，反应时间短，操作简单，收率高，所得到的乌拉立肽杂质HPLC纯度达到99.5％以上，可以作为标准品用于乌拉立肽制备过程中的杂质研究。 【EN】The invention belongs to the technical field of medicines, and particularly discloses a urotropine impurity, which is a main impurity component in the later stage of urotropine purification by finding that urotropine methionine oxide penetrates through the whole urotropine purification process through sample tracking and monitoring. The preparation method has the advantages of short reaction time, simple operation and high yield, and the obtained ularitide impurity HPLC purity reaches more than 99.5 percent and can be used as a standard substance for impurity research in the ularitide preparation process.

摘要：【中文】本发明提供了一种异丙托溴铵晶体的制备方法。具体步骤为：将异丙托溴铵加入到良性溶剂中后，加热搅拌溶解，溶液澄清后，滴加不良溶剂，通过程序降温析晶得到高纯度的异丙托溴铵晶体。本发明所述的制备方法操作简单、产品收率高、纯度高，并且该晶体具有较好的溶解性与化学稳定性，适合于工业化生产。 【EN】The invention provides a preparation method of ipratropium bromide crystals. The method comprises the following specific steps: adding ipratropium bromide into a benign solvent, heating, stirring and dissolving, after the solution is clarified, dropwise adding a poor solvent, and performing temperature reduction and crystallization by a program to obtain a high-purity ipratropium bromide crystal. The preparation method provided by the invention is simple to operate, high in product yield and high in purity, and the crystal has good solubility and chemical stability and is suitable for industrial production.

摘要：【中文】本发明提供了一种异丙托溴铵一水合物及其制备方法。具体步骤为：将异丙托溴铵加入到良性溶剂中后，加热搅拌溶解并滴加一定量的纯化水，溶液澄清后，滴加不良溶剂，通过程序降温析晶得到高纯度的异丙托溴铵一水合物。本发明所述的制备方法操作简单、产品收率高、纯度高，并且本发明提供的异丙托溴铵一水合物具有较好的溶解性与化学稳定性，适合于工业化生产。 【EN】The invention provides ipratropium bromide monohydrate and a preparation method thereof. The method comprises the following specific steps: adding ipratropium bromide into a benign solvent, heating, stirring, dissolving, dropwise adding a certain amount of purified water, clarifying the solution, dropwise adding a poor solvent, and performing temperature reduction and crystallization by a program to obtain the high-purity ipratropium bromide monohydrate. The preparation method provided by the invention is simple to operate, high in product yield and high in purity, and the ipratropium bromide monohydrate provided by the invention has better solubility and chemical stability, and is suitable for industrial production.

摘要：【中文】本发明属于医药技术领域，具体公开了一种多肽制备纯化方法。本发明在乌拉立肽制备纯化过程中使用了抑制甲硫氨酸氧化的方法，使得纯化后的乌拉立肽精制品纯度高达99.90％，甲硫氨酸氧化杂质肽控制在0.1％内。 【EN】The invention belongs to the technical field of medicines, and particularly discloses a method for preparing and purifying polypeptide. The method for inhibiting methionine oxidation is used in the process of preparing and purifying the ularitide, so that the purity of the purified ularitide refined product is up to 99.90 percent, and the methionine oxidation impurity peptide is controlled within 0.1 percent.

摘要：【中文】本发明属于医药领域，主要涉及一种丹皮酚包合物的制备方法，具体制备方法为：从牡丹皮药材中用水蒸气蒸馏法提取丹皮酚溶液，将一定量的β‑环糊精直接加入到丹皮酚溶液中，搅拌，形成‑β环糊精的饱和溶液，搅拌包合一段时间后，将包合溶液低温冷藏，过滤干燥，即可得到包合物。与常规的丹皮酚包合工艺相比，本包合工艺简便快速，省略了丹皮酚溶液过夜冷藏析晶的步骤，节约了时间，提高了包合效率，丹皮酚的包合率大于80％。 【EN】The invention belongs to the field of medicine, and mainly relates to a preparation method of a paeonol inclusion compound, which comprises the steps of extracting paeonol solution from a tree peony bark medicinal material by a steam distillation method, directly adding a certain amount of β -cyclodextrin into the paeonol solution, stirring to form saturated solution of- β cyclodextrin, stirring for inclusion for a period of time, refrigerating the inclusion solution at low temperature, filtering and drying to obtain the inclusion compound.

摘要：【中文】本发明涉及药物技术领域，具体涉及一种达沙替尼晶型及制备方法。本发明的达沙替尼晶型物的粉末衍射图谱中2θ在5.8±0.2°，7.2±0.2°，14.4±0.2°，16.0±0.2°处有衍射峰。X‑射线单晶衍射图谱显示本发明制备的晶型为达沙替尼乙醇溶剂合物晶，型纯度高，稳定性好，溶解度优良，尤其在溶出实验中展现出了优良的溶出性能，其制备过程易于工业化，具有广阔的应用前景。 【EN】The invention relates to the technical field of medicines, and particularly relates to a dasatinib crystal form and a preparation method thereof. In the powder diffraction pattern of the dasatinib crystal form substance, diffraction peaks exist at positions of 5.8 +/-0.2 degrees, 7.2 +/-0.2 degrees, 14.4 +/-0.2 degrees and 16.0 +/-0.2 degrees of 2 theta. The X-ray single crystal diffraction pattern shows that the crystal form prepared by the invention is dasatinib ethanol solvate crystal, the crystal form purity is high, the stability is good, the solubility is excellent, the excellent dissolution performance is particularly shown in a dissolution experiment, the preparation process is easy to industrialize, and the application prospect is wide.

摘要：【中文】本发明涉及药物技术领域，具体涉及技术领域一种达沙替尼新晶型及制备方法。本发明的达沙替尼新晶型的粉末衍射图谱中2θ在5.8±0.2°，6.9±0.2°，12.5±0.2°，13.2±0.2°，13.7±0.2°处有衍射峰。通过本发明制备的达沙替尼新晶型纯度高，稳定性好，溶解度优良，尤其在溶出实验中展现出了优良的溶出性能，其制备过程易于工业化，具有广阔的应用前景。 【EN】The invention relates to the technical field of medicines, in particular to a novel dasatinib crystal form and a preparation method thereof. In the powder diffraction pattern of the novel dasatinib crystal form, diffraction peaks exist at positions of 5.8 +/-0.2 degrees, 6.9 +/-0.2 degrees, 12.5 +/-0.2 degrees, 13.2 +/-0.2 degrees and 13.7 +/-0.2 degrees. The novel dasatinib crystal form prepared by the method has high purity, good stability and excellent solubility, particularly shows excellent dissolution performance in a dissolution experiment, is easy to industrialize in the preparation process, and has wide application prospect.

摘要：【中文】本发明属于医药制剂技术领域，具体涉及了一种CYP17抑制剂片及其制备方法，该片剂将醋酸阿比特龙和共聚维酮用热熔挤出机在115℃‑125℃加热熔融挤出，制备固体分散体，再将挤出物粉碎后与填充剂、崩解剂混合，然后加入润滑剂混合，压片而成。该片剂溶出速度快，稳定性、工艺重现性均较好，适合于规模化生产。 【EN】The invention belongs to the technical field of pharmaceutical preparations, and particularly relates to a CYP17 inhibitor tablet and a preparation method thereof. The tablet has the advantages of high dissolution rate, good stability and process reproducibility, and suitability for large-scale production.