10YR企业会员
发布人:长沙上禾生物科技有限公司
发布日期:2026/7/18 21:25:18
公司官网 http://www.staherb.com/ 资质:HALAL, KOSHER等认证
☎:19573130018 杨经理(微信同号)
工艺路线总览:
上禾生物育亨宾提取物生产分两条主线:
标准化树皮提取物(Yohimbine 2%~20% HPLC,比例 4:1~20:1)——树皮前处理 → 酸醇提取 → 碱沉/酸沉除杂 → 大孔吸附树脂富集 → 喷雾干燥;
高纯育亨宾碱单体 / 盐酸育亨宾(≥98% HPLC)——标化提取物经大孔/离子交换树脂深度纯化、硅胶/ODS柱层析、酸转化成盐、有机溶剂重结晶精制。
关键生产工序:
① 原料前处理(关键控制点)
选用喀麦隆、刚果、加蓬等西非/中非产区的育亨宾树(Pausinystalia yohimbe)干燥树皮,优选15~20年生成年树皮,入厂检测育亨宾碱基线≥0.8%~1.5% DW(拒收<0.5%~0.8%),严控水分≤10%、霉变、重金属及非Pausinystalia树皮混入,附CITES/当地合法采伐文件。
干树皮除杂 → 粉碎过20~40目筛(过细易带入木质素/树脂杂质堵柱,过粗生物碱提取不尽);
育亨宾碱具吲哚喹啉结构,对热、光、强酸强碱敏感,前处理与存储须避光、低温、控pH。
② 酸醇提取(Acid-Alcohol Extraction —— 生物碱溶出核心)
育亨宾在植物中以生物碱盐或游离弱碱存在,难溶于水,易溶于醇及酸水溶液。采用 50%~90% 食品级乙醇 + 0.05~0.1 mol/L 稀硫酸/盐酸 调pH 3~4 的酸醇混合溶剂,料液比1:5~1:10,70~85℃ 回流或超声辅助提取 2~3次(1~2h/次),利用H⁺使生物碱成盐增溶。
合并提取液 → 板框/离心过滤 → 减压浓缩(≤60℃、N₂保护) 回收乙醇至适当比重(1.10~1.20),防热敏降解;也可用超临界CO₂(加夹带剂)绿色提取但成本高。
③ 除杂——碱沉/酸沉与脱脂(Impurity Removal)
浓缩液调碱沉杂:用氨水、碳酸钠等弱碱调pH 8~10,使部分伴生杂质(树脂、鞣质、色素)沉淀或使游离生物碱析出初分离,过滤收集沉淀或上清;
酸溶/水沉:沉淀用稀酸水溶解 → 过滤去不溶物(木质素、蜡质)→ 滤液备用;或浓缩液加水水沉除去醇溶多糖/蛋白/胶体;
必要时用石油醚/正己烷脱脂除去叶绿素与油脂。
④ 纯化富集——大孔吸附/离子交换树脂(Core Purification)
酸水溶液稀释至适宜浓度上大孔吸附树脂(AB-8、D101、LX-18、LS-300等)或弱酸性阳离子交换树脂:
水洗除糖、有机酸、水溶性色素;
用 10%~50% 乙醇/甲醇 洗去黄酮、部分弱碱杂质与低极性伴生物;
用 70%~80% 乙醇(或调pH 8~10的碱性醇) 梯度洗脱收集育亨宾及伴生生物碱流份(HPLC跟踪,育亨宾转移率70%~80%)。
为分离伪育亨宾、α/β-育亨宾、柯楠碱等立体异构体,可二次过柱或采用ODS反相/硅胶柱层析精细分离。
⑤ 浓缩与标化干燥
洗脱液低温(≤50℃)减压浓缩除醇/水 → 喷雾干燥(进风150~160℃,出风70~80℃,加抗氧壁材)或真空/冷冻干燥得棕黄至棕褐色粉末(2%~20% Yohimbine)。
⑥ 高纯单体精制(Yohimbine Base ≥98% / Yohimbine HCl ≥98%)
路线A(游离碱重结晶):标化提取物溶于热无水乙醇/甲醇/乙酸乙酯,加0.1%~0.5% 活性炭脱色(40~60℃搅拌),热滤 → 滤液低温(2~5℃)缓慢析晶 → 过滤得粗结晶 → 重复乙酸乙酯/乙醇-水重结晶2~3次 → 真空干燥(≤40℃)得白色至类白色育亨宾碱(≥98% HPLC),单杂(伪/α/β型)<0.1%~0.5%。
路线B(盐酸育亨宾成盐):游离碱或高纯提取物溶于少量稀盐酸-乙醇溶液,调pH 3~4 成盐 → 浓缩 → 乙醇-水/丙酮-水体系重结晶 → 过滤得盐酸育亨宾(Yohimbine Hydrochloride,≥98%~99% 白色结晶),水溶性显著提升;
全程避光、控湿(生物碱盐引湿)、充氮防氧化变色。
⑦ 质控与包装
检测:HPLC测育亨宾(主峰及伪育亨宾、α/β-育亨宾、柯楠碱等有关生物碱)、手性纯度评估;UV辅助;检查干燥失重、炽灼残渣、重金属(Pb≤1~10ppm等)、酸根(Cl⁻/SO₄²⁻)残留、溶剂残留(乙醇/甲醇/乙酸乙酯)、微生物;
粉末/晶体:内双层PE+棕色玻璃瓶/铝箔袋(充氮/真空);严格避光、2~8℃冷藏或-20℃冷冻(生物碱光敏易降解,盐酸盐引湿);保质期24个月;
年产能:育亨宾树皮提取物数十吨级(2%~20%),高纯育亨宾碱/盐酸盐因原料含量极低、分离难,按订单百克至公斤级定制;
质量体系:ISO 9001 / GMP / ISO 22000 / HALAL / KOSHER;可提供COA、MSDS、典型HPLC色谱图、CITES合规文件。

Process Route Overview:
Staherb produces two main categories of Yohimbine Extract:
Standardized Bark Extract (Yohimbine 2%~20% HPLC, Ratio 4:1~20:1) — Bark pre-treatment → Acid-alcohol extraction → Alkali/acid precipitation → Macroporous/Ion-exchange resin enrichment → Spray drying.
High-purity Yohimbine Base / Yohimbine Hydrochloride (≥98% HPLC) — Standardized extract further purified via deep macroporous/IEX resin, silica/ODS column chromatography, salification (HCl), and organic solvent recrystallization.
Key Production Steps:
Step
Description
① Raw Material Pre-treatment
Source: Dried bark of Pausinystalia yohimbefrom Cameroon, Congo, Gabon (West/Central Africa), prefer 15–20 yr mature bark. Test: Yohimbine baseline ≥0.8%~1.5% DW (reject<0.5%~0.8%), moisture ≤10%, mold, heavy metals, non-Pausinystaliaadmixture, with CITES/local legal harvest docs. Debris removed → milled 20–40 mesh (too fine introduces lignin/resin clogging; too coarse poor alkaloid extraction). Yohimbine (indole-quinolizidine) is light/heat/extreme acid-base sensitive; pre-treatment/storage requires light protection, low-temp, pH control.
② Acid-Alcohol Extraction (Core Alkaloid Solubilization)
Yohimbine exists as alkaloidal salts or free weak base, poorly water-soluble but soluble in alcohols/acids. Extract with 50%–90% food-grade EtOH + 0.05–0.1 mol/L H₂SO₄/HCl (pH 3–4), 1:5–10 w/v, 70–85℃ reflux or ultrasound-assisted 2–3× (1–2h). H⁺ converts base to salt for solubilization. Combine → filter → vacuum conc. (≤60℃, N₂) to rel. dens. 1.10–1.20. Alternately supercritical CO₂ (with entrainer) for green extraction at higher cost.
③ De-impurity: Alkali/Acid PPT & Degreasing
Alkalinization: Adjust conc. to pH 8–10 with NH₄OH, Na₂CO₃ to precipitate impurities (resins, tannins, pigments) or precipitate free alkaloid for crude separation → filter.
Acid re-dissolution / Water precipitation: Precipitate redissolved in dilute acid → filter remove lignin/waxes; or concentrate diluted with water to water-precipitate polysaccharides/proteins/colloids.
Optionally petroleum ether/n-hexane degreasing to remove chlorophyll/fats.
④ Purification — Macroporous / Ion-Exchange Resin (Core)
Diluted acid soln loaded onto macroporous (AB-8, D101, LX-18, LS-300) or weak acid cation-exchange resins: water wash → 10%–50% EtOH/MeOH remove flavonoids, weak alkaloids, low-polar impurities → 70%–80% EtOH (or pH 8–10 alk. alcohol) gradient elution to collect Yohimbine & accompanying alkaloids (HPLC tracked, recovery 70%–80%).
For separating Pseudoyohimbine, α/β-Yohimbine, Corynanthine, secondary column or ODS/silica gel chromatography may be used.
⑤ Concentration & Standardized Drying
Eluate conc. under reduced pressure (≤50℃) → spray-dry (inlet 150–160℃, outlet 70–80℃, with antioxidant wall material) or vacuum/freeze-dried to brownish-yellow to brown powder (2%~20% Yohimbine).
⑥ High-purity Monomer (≥98% Base / HCl)
Route A (Base Recrystallization): Standardized extract dissolved in hot anhydrous EtOH/MeOH/EA, add 0.1%–0.5% activated carbon (40–60℃ stir) → hot filter → slow recrystallization at 2–5℃ → filter crude → repeat EA/EtOH-H₂O recrystallization 2–3× → vacuum dry (≤40℃) to white/off-white Yohimbine base (≥98% HPLC), related (Pseudo/α/β)<0.1%–0.5%.
Route B (Yohimbine HCl Salification): Base/high-pure extract dissolved in dilute HCl-EtOH, adjust pH 3–4 to form salt → conc. → recrystallized from EtOH-H₂O / acetone-H₂O → filter to Yohimbine Hydrochloride (≥98%~99% white crystals) with improved water solubility. Process light/humidity (hygroscopic salt) / N₂ protected.
⑦ QC & Packaging
Assay by HPLC (Yohimbine, Pseudoyohimbine, α/β-Yohimbine, Corynanthine & related alkaloids), chiral purity assessment; UV auxiliary; LOD, heavy metals (Pb≤1–10ppm), acid radical (Cl⁻/SO₄²⁻) residue, residual solvents (EtOH/MeOH/EA), microbes. Powder/crystals: double PE + amber glass/foil (N₂/vac); strictly light-protected, 2–8℃ or -20℃ (alkaloids light-degradable, HCl salt hygroscopic); shelf life 24 mos.
Capacity: Dozens of tons/year bark extract (2%~20%), high-pure Yohimbine base/HCl made-to-order in hundreds-of-grams to kg scale due to low baseline and separation difficulty.
Certifications: ISO 9001 / GMP / ISO 22000 / HALAL / KOSHER; COA, MSDS, typical HPLC chromatograms, CITES compliance docs provided.
育亨宾碱/盐酸育亨宾属单萜吲哚生物碱,对光、热(>60℃长时)、强酸强碱、金属离子敏感,易降解变色(褐变);提取宜酸醇控温≤85℃(优选70~80℃)、弱酸pH 3~4、N₂保护、避光;
伴生异构体(伪/α/β-育亨宾)结构与育亨宾极近似(手性差异),高纯分离极度依赖制备色谱(硅胶/ODS/HPLC)与多次重结晶,成本高、得率极低;
酸醇提取含腐蚀性与易燃溶剂(乙醇+无机酸),须防腐蚀与残留(终产品酸根/溶剂严控);
高纯单体/盐酸盐具强药理活性、引湿性与光敏性,2~8℃充氮冷藏/-20℃冷冻、开封速用;在中/美/欧多国属处方药/受管制物质,严禁普通食品/补剂/化妆品添加,仅限医药处方、科研、法规明示允许区使用。
至此,长沙上禾生物全部15+款核心植物提取物/活性单体(……育亨宾提取物/育亨宾碱/盐酸育亨宾)的六大维度均已完整覆盖。
公司官网 http://www.staherb.com/ 资质:HALAL, KOSHER等认证
☎:19573130018 杨经理(微信同号)
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