CN112266941A - 酶碱结合生产小分子果胶的方法 - Google Patents
酶碱结合生产小分子果胶的方法 Download PDFInfo
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- CN112266941A CN112266941A CN202011064484.8A CN202011064484A CN112266941A CN 112266941 A CN112266941 A CN 112266941A CN 202011064484 A CN202011064484 A CN 202011064484A CN 112266941 A CN112266941 A CN 112266941A
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- pectin
- solution
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- molecular
- alkali
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Abstract
本发明公开了一种酶碱结合法精确控制小分子果胶分子量和酯化度的生产方法。该工艺先用果胶裂解酶将果胶分子量裂解至目标分子量,再加入调pH值范围在8‑12的碱溶液将小分子果胶的酯化度降低到目标酯化度,脱酯完成后加入酸经中和、澄清过滤、酒精沉淀、洗涤、干燥、粉碎,获得了水溶性好,纯度高、透明度好、分子量大小可控且分子量分布范围窄、酯化度高低可控到适用于不同功能应用的小分子果胶。该工艺和单一的碱法或酶法相比,产品的分子量分布范围更窄,生产工艺更简单。本方法得到的小分子果胶粉可用于食品、保健品、特殊医学配方食品、药品等原料。同时该方法工艺流程短,生产成本低,产业化能力强,适合大规模生产。
Description
技术领域
本发明涉及高分子化合物水解领域,尤其涉及一种小分子果胶的酶碱结合制备方法
背景技术
天然果胶是植物中的一种酸性多糖物质,为稍带酸味的白色至淡黄色粉末,具有水溶性, 分子量约5万~30万。现今市场上通常将高分子果胶作为食品添加剂用于食品加工行业,如 胶凝剂、增稠剂、稳定剂、悬浮剂、乳化剂等。另外,天然果胶还可用于化妆品,对保护皮 肤、防止紫外线辐射、冶疗创口、美容养颜,保护胃肠都有一定作用。但是,天然果胶是多 聚糖长链碳水化合物,水溶性差,口感不好,不易吸收。因此,高分子果胶在生物学活性方 面的应用受到限制。
小分子果胶是从天然果胶长链切断并降低酯化度的短链低酯化度的半乳糖醛酸及盐,小 分子果胶易溶解、分子量小到可直接吸收进入血液循环,果胶属水溶性膳食纤维,而膳食纤 维进入血液循环对健康是质的变化:小分子果胶对癌症的关健蛋白Galectin-3有很强的络合 吸附作用,可阻止癌细胞的聚集、生长和转移,阻止肿瘤细胞的营养吸收(Galectin-3对癌细 胞有聚集、吸收养分、着床、生长和转移的能力,是癌症的元凶),小分子果胶可特异性的 杀伤已突变肿瘤细胞,使突变细胞活性降低,并在未形成之前即被清除,小分子果胶也有直 接增强免疫功能,调节和增加单核细胞细胞毒,增强巨噬细胞的吞噬功能,它的成分 rhamnogalacturonan能提高CD3+T细胞和NK细胞的细胞毒活性,增强T细胞的活动能 力,从而清除肿瘤细胞,小分子果胶能将免疫系统从对细菌感染的反应转到一种更为平衡的 系统,这个系统能主动地寻找并清除癌细胞和病毒感染细胞,并刺激体内免疫系统寻找破坏 突变细胞,抑制TH@对抗过敏源,控制病毒细菌传染,帮助TH1清除有毒物质及突变细胞, 增强机体免疫功能,对维持一个平衡的免疫系统起到很重要的作用,所以小分子果胶有很好 预防癌症的作用,并在放化疗中有很好的增加疗效和减少毒副作用。
小分子果胶直接结合血液中的有毒重金属(铅、铬、镉、汞、砷等),有选择性的且以缓 慢、温和的方式排泄有毒重金属,从而减少其对身体的毒性,但对人体有益的铁、钠、钙、锌、镁、硒等金属元素无排泄作用,由于能有效排除人体中有害重金属和毒素,具有去除色斑、黄褐斑,修复疤痕的由内而外的美容功能。
小分子果胶可延缓糖和脂肪在消化道内的吸收,影响胆酸的代谢,间接改变了脂质代谢 酶的活性,还能促进糖和脂肪在体内的代谢,从而降低血糖和血脂,在吸收进入血液循环后, 能在体内促进肝脏及其它器官中的糖和脂肪分解酶的活性,并降低肝脏及其他器官中的糖和 脂肪合成酶的活性,从而达到降糖、降脂减少糖尿病和脂肪肝的目的。
小分子果胶具有很好的解酒护肝功能。
小分子果胶可有效改善胃肠道功能,有利于益生菌生长,抑制有害菌生长,对解决便秘 有很好功效。
小分子果胶能有效护肤持水,防辐射。
小分子果胶能有效预防脑中风。
发明内容
本发明的目的是提供一种利用酶碱组合水解结合酒精纯化的方法制取低酯化度、高半乳 糖醛酸含量窄分子量分布的小分子果胶制备工艺。运用酶碱结合技术和酒精纯化技术相结合 的制备工艺,工艺过程中控制酯化度和水解程度,酶解和酒精纯化控制分子量分布范围,并 通过真空干燥技术回收酒精,减少了环境污染并降低了生产成本,获得的产品水溶性好,分 子量可控且分布范围窄,酯化度根据应用功能要求不同高低可控,产品对抑制肿瘤及解酒和 除铅效果好。该发明对于拓展果胶在医药、保健品、功能性食品、持医食品行业的应用意义 重大。
本发明的目的是通过如下技术方案实现的:一种酶碱结合生产小分子果胶的方法,包括如下 步骤:
(1)先用果胶裂解酶将高分子果胶裂解至分子量至1500-50000Da的小分子果胶:
在浓度为3-12kg/100L、PH值为2.5-5.5的高分子果胶溶液中加入质量为高分子果胶粉 干重0.05%-2.0%的果胶裂解酶,在20-50℃温度下水解0.5-10小时后冷却至室温获得分子量 至1500-50000Da的小分子果胶。其中,高分子果胶溶液的浓度为3-12kg/100L,果胶裂解酶 的加入质量为高分子果胶干重的0.05%-2.0%。
(2)利用碱溶液对小分子果胶进行脱酯控制果胶的酯化度为2%-45%:
往步骤(1)水解得到的溶液加入碱性溶液,调节PH值至8-12进行脱酯,脱酯时间为0.25-10小时,用酸性溶液将溶液的pH调节至5.5-7.0,过滤去除不溶性固体得果胶透明溶液。
(3)往步骤(2)获得的透明果胶溶液中加入质量百分数为85%-95%酒精进行沉淀,然 后过滤,滤渣用质量百分数为85-95%的酒精进行洗涤、离心脱水,干燥、粉碎、过80目筛 后制得小分子果胶。
进一步地,所述的小分子果胶包括部分甲酯化的低聚半乳糖醛酸和半乳糖醛酸盐,包括 钠、钾、钙、铁、锌和氨盐。
进一步地,获得的小分子果胶的分子量在1500-50000Da。
进一步地,所述高分子果胶溶液通过如下方法制得:将高分子果胶粉过40-80目筛后在 搅拌下加入质量为高分子果胶粉干重8-30倍的无离子水中溶解,加入碱性溶液调PH至2.5-5.5 得到浓度为3-12kg/100L的高分子果胶溶液。
进一步地,所述高分子果胶溶液通过如下方法制得:将清洗干净的含果胶原料粉碎至 20-150目,搅拌下加入含果胶原料重量15-50倍的无离子水中,加入硝酸调PH值至0.5-2.0, 加温60-95℃提取果胶0.5-10小时,过滤除去残渣得果胶溶液;往果胶溶液中加入氨水或NaOH 或碳酸钠中和至PH值2.5-5.5,果胶溶液冷却至20-50℃,精滤至溶液透明并浓缩至浓度为 3-12kg/100L得果胶浓缩液。所述含果胶原料包括柑橘、柠檬、橙、桔、柚、苹果、等水果 皮或果皮渣。
进一步地,所述高分子果胶粉通过如下方法制备得到:将清洗干净的葵花盘粉碎至20-150 目,加入干葵花盘重量15-50倍的无离子水中,加入干葵花盘重量5%-15%草酸铵,用草酸调 PH值至4.0-5.0,加温60-95℃提取果胶0.5-10小时,过滤除去残渣得果胶溶液;果胶溶液冷 却至20-50℃,精滤至溶液透明并浓缩至浓度为3-12kg/100L,得果胶浓缩液。
进一步地,所述碱性溶液为氢氧化钠溶液或氢氧化钾溶液或氢氧化钠和氢氧化钾的混合 溶液,酸性溶液为盐酸或硝酸溶液。
本发明还提供了一种小分子果胶在制备食品、保健品、特殊医学配方食品、药品中的应 用。
本发明的有益效果是:本发明方法运用酶碱组合技术和酒精纯化技术相结合的制备工艺, 利用果胶酶在碱液中失活的特点,可以精准的控制分子量,根据碱液的PH值(8-12)高低可 精确控制酯化度,减少了专利号:ZL201310380333.7工艺中双酶法需要加温灭酶的复杂工艺, 工艺过程中控制酯化度和水解程度,酶水解和酒精纯化控制分子量分布范围,产品得率高。 而且获得的产品水溶性好,溶解后透明度高,根据应用功能的不同分子量大小可控且分布范 围窄,酯化度按功能要求高低可精确控制,抑制肿瘤及解酒和除铅效果好。另外,本方法中 还可以通过真空干燥技术回收酒精,减少了环境污染并降低了生产成本,同时该方法工艺流 程短,生产成本低,产业化能力强,适合大规模生产。
附图说明
图1为实施例1制备的小分子果胶高效液相凝胶色谱图;
图2为实施例2制备的小分子果胶高效液相凝胶色谱图;
具体实施方式
本发明提供了酶碱结合生产小分子果胶的方法,该方法可以直接用果皮渣提取获得果胶 溶液或将高分子果胶搅拌下溶解于无离子水中得到果胶溶液,加入果胶裂解酶,控制时间、 温度、酶的量和PH值,将果胶降解成可控分子量并集中峰值的小分子果胶,加入一定的碱 量调整PH值,在碱性溶液中可纯化果胶裂解酶,控制分子量不会继续降低,利用果胶在碱 性中易脱酯的特点,通过加入定量的碱可精确控制果胶的酯化度,然后中和,精滤澄清,加 入酒精沉淀,分离除去酒精液,再用酒精清洗果胶,分离、干燥、粉碎后可得所需要精确控 制酯化度和分子量的小分子果胶,通过该制备方法得到的小分子果胶粉符合美国USP30标准, 提高了小分子果胶提取的纯度,同时该方法工艺流程短,生产成本低,产业化能力强,适合 大规模生产。
本发明中测定分子量的方法为高效液相凝胶色谱法,将分子量的分布范围分为三大部分: 20000D以上,20000~6000D之间和6000D以下。具体的分析条件为:TSKgelG2000SWXL 色谱柱,分子量分级范围100~10000,流动相:50mmol/L的醋酸铵缓冲液,示差折光检测 器,流速0.5ml/min,进样量10ul,柱温30℃。
下面,结合具体实施例对本发明作进一步说明。
实施例1
称取干的葵花盘20公斤粉碎至30目,加入到20倍70度热水中搅拌清洗30分钟后压榨 过滤并用70度热水反洗至滤出液清,清洗干净并榨干的葵花盘加入至300L无离子水中,加 温至85度,加好后溶液总400L,加入草酸铵2.5公斤并用草酸调PH=4.5,85度搅拌反应提 取果胶2小时,过滤,滤液精滤至透明,冷却至50℃,用0.05微米膜设备浓缩至浓度为6kg/100L,得浓缩液58L,加入果胶酶18.9g搅拌反应4.0小时降解,加入KOH调PH=11.2 脱酯反应4.0小时,加硝酸中和至PH=6.5,用0.2微米滤膜过滤得透明果胶溶液,再加入质 量百分浓度为90%酒精进行沉淀并过滤;滤渣用95%的酒精进行反复洗涤2次后离心脱水,粉碎,真空干燥并回收酒精;干燥后果胶研磨,得粉状小分子果胶提取物3.10KG,得率为15.5%。产物平均分子量为8947道尔顿,酯化度9.2%,其色谱图如图1所示,结果如表1 所示。产品透光度大于92%,溶解速度快,属速溶产品。
表1实施例1色谱结果
Name | Retention Time | Mn | Mw | MP | Polydispersity | %Area | Mz+1 | Mz | Area | %Amount |
Peak3 | 11.942 | 8947 | 11642 | 14066 | 1.301139 | 100.00 | 17353 | 14512 | 196410502 |
实施例2
称取干的苹果皮楂20公斤粉碎至60目,加入到30倍70度热水中搅拌清洗30分钟后压 榨过滤并用70度热水反洗至滤出液清,清洗干净并榨干的苹果皮楂搅拌下加入90度的无离 子水中,加好后溶液总400L,加入硝酸调PH=0.5,保持温度提取果胶3小时,过滤,滤液 加NaOH调PH=3.5,冷却至40度,用0.2微米孔膜设备过滤得到透明果胶液,再用0.05微米膜设备浓缩至浓度为10kg/100L,得26L浓缩液,加入果胶酶30g搅拌反应4.5小时降解,加入KOH调PH=12脱酯反应4.5小时,加硝酸中和至PH=6.5,用0.2微米滤膜过滤得透明 果胶溶液,再加入质量百分浓度为90%酒精进行沉淀并过滤;滤渣用95%的酒精进行反复洗涤2次后离心脱水,粉碎,真空干燥并回收酒精;干燥后果胶研磨,得粉状小分子果胶提取物2.60KG,得率为13.0%。产物平均分子量为5638道尔顿,酯化度2.2%,其色谱图如图2 所示,结果如表2所示。产品透光度大于94%,溶解速度快,属速溶产品。
表2实施例2色谱结果
Name | Retention Time | Mn | Mw | MP | Polydispersity | %Area | Mz+1 | Mz | Area | %Amount |
Peak3 | 12.662 | 5638 | 6356 | 5825 | 1.127286 | 100.00 | 7946 | 7145 | 80417602 |
实施例3
称取10公斤已清洗柠檬皮渣,粉碎过30目筛,搅拌下加入300公斤75℃无离子水中, 调节水温70℃,加入硝酸调PH=0.8,保持温度提取果胶3小时,过滤,滤液加NaOH调PH=3.5, 冷却至30度,用0.2微米孔膜设备过滤得到透明果胶液,再用0.05微米膜设备浓缩至浓度为 8kg/100L,得40L浓缩液,加入果胶酶11.55g搅拌反应4.5小时降解,加入KOH调PH=11.2 脱酯反应4.5小时,加硝酸中和至PH=6.5,用0.2微米滤膜过滤得透明果胶溶液,再加入质 量百分浓度为90%酒精进行沉淀并过滤;滤渣用95%的酒精进行反复洗涤2次后离心脱水, 粉碎,真空干燥并回收酒精;干燥后果胶研磨,得粉状小分子果胶提取物2.89KG,得率为 28.9%。产物平均分子量为7800道尔顿,酯化度7.8%。产品透光度大于94%,溶解速度快, 属速溶产品。经药理实验,其抑制肿瘤、排铅效果好,降血糖血脂明显,护扶持水,防辐射, 预防脑中风效果优。
实施例4
称取10公斤已清洗柑橘皮渣,粉碎过150目筛,搅拌下加入300公斤75℃去离子水中, 调节水温90℃,加入硝酸调PH=2,保持温度提取果胶10小时,过滤,滤液加NaOH调PH=5.5, 冷却至温度50度,用0.2微米孔膜设备过滤得到透明果胶液,再用0.05微米膜设备浓缩至浓 度为8kg/100L,得30L浓缩液,加入果胶酶0.5g搅拌反应4.5小时降解,加入KOH调PH=11.2 脱酯反应3.5小时,加硝酸中和至PH=6.5,用0.2微米滤膜过滤得透明果胶溶液,再加入质 量百分浓度为90%酒精进行沉淀并过滤;滤渣用95%的酒精进行反复洗涤2次后离心脱水, 粉碎,真空干燥并回收酒精;干燥后果胶研磨,得粉状小分子果胶提取物2.09KG,得率为 20.9%。产品品质同实施例3。
上述方法同样适用于柑橘、柠檬、橙、桔、柚、苹果、等水果皮或果皮渣以及延伸甜菜 渣,淀粉渣,蚕粪渣,南瓜皮等含果胶原料去制备小分子果胶。
实施例5
称取高分子果胶粉10KG,搅拌下加入125L去离子水中,温度20℃,加入200g的果胶裂解酶,加氢氧化钠溶液调节高分子果胶溶液的pH值到2.5,机械搅拌下20℃温度下水解280min,再加氢氧化钠溶液调pH至11.2脱脂6.0h,过滤去不溶性固体得透明果胶溶液;用盐酸调PH=6.2,再加入质量百分浓度92%酒精进行沉淀并过滤;滤渣用95%的酒精进行反复 洗涤2次后离心脱水,粉碎,真空干燥并回收酒精;干燥后果胶研磨,得粉状小分子果胶8.6KG, 得率为86%。产物平均分子量为15000道尔顿,酯化度8.2%。产品品质同实施例3。
实施例6
称取高酯果胶粉10KG,搅拌下加入150L去离子水,温度50℃,调节高分子果胶溶液的pH值到5.5,机械搅拌下加入2g的果胶裂解酶,机械搅拌下50℃温度下水解180min,降 温至30度,加氢氧化钠溶液调pH至10.2脱脂3h,过滤去不溶性固体得透明果胶溶液;加 盐酸调PH=6.0,再加入质量百分浓度92%酒精进行沉淀并过滤;滤渣用95%的酒精进行反复洗涤2次后离心脱水,粉碎,真空干燥并回收酒精;干燥后果胶研磨,得粉状小分子果胶8.9KG, 得率为89%。产物的平均分子量为26500道尔顿,酯化度26%,经药理实验,其解酒、醒酒、 改善胃肠道功能效果优。
实施例7
称取高酯果胶粉10KG,搅拌下加入至330L去离子水中,温度50℃,调节高分子果胶溶液的pH值到5.5,机械搅拌下加入200g的果胶裂解酶,机械搅拌下50℃温度下水解30min,降温至30度,加氢氧化钠溶液调pH至9.2脱脂3.0h,过滤去不溶性固体得透明果胶溶液; 加盐酸调PH=5.6,再加入质量百分浓度85%酒精进行沉淀并过滤;滤渣用95%的酒精进行反复洗涤2次后离心脱水,粉碎,真空干燥并回收酒精;干燥后果胶研磨,得粉状小分子果胶8.8KG,得率为88%。产物的平均分子量为18000道尔顿,酯化度31%.经药理实验,其美容养颜、护肤持水、防辐射功能效果优。
实施例8
称取高分子果胶粉10kg,搅拌下加入至80L无离子水中,温度45℃,调节高分子果胶溶 液的pH值到3,机械搅拌条件下加入2g的果胶裂解酶,机械搅拌下45℃温度下水解600min; 冷却至室温,加氢氧化钾溶液调pH至8脱脂3h,过滤去不溶性固体得透明果胶溶液;加盐 酸调节PH至6.5,再加入质量百分浓度95%酒精进行沉淀并过滤;滤渣用85%的酒精进行反 复洗涤2次后离心脱水,粉碎,真空干燥并回收酒精;干燥后果胶研磨,得粉状改性果胶提 取物88g,得率为88%。产物的平均分子量为35000道尔顿,酯化度41%。
实施例9
称取高分子果胶粉10kg,搅拌下加入300L水中,温度25℃,调节高分子果胶溶液的pH 值到3,机械搅拌条件下加入200g的果胶裂解酶,25℃温度下水解600min;,加氢氧化钾溶 液调pH至11.8脱脂6h,过滤去不溶性固体得透明果胶溶液;加盐酸调节PH至6.5,再加入质量百分浓度95%酒精进行沉淀并过滤;滤渣用85%的酒精进行反复洗涤2次后离心脱水,粉碎,真空干燥并回收酒精;干燥后果胶研磨,得粉状小分子果胶8.5kg,得率为85%。产 物的平均分子量为1800道尔顿,酯化度45%。
本发明方法通过酶碱组合控高分子果胶的酯化度和水解程度,酶水解和酒精纯化控制分 子量分布范围,获得了水溶性好,分子量分布范围窄,酯化度适中可控制的小分子果胶,制 得的小分子果胶适用于作为抑制肿瘤、降低放化疗毒副作用﹑降血糖血脂、提高免疫力、改 善胃肠道功能、解除重金属、解酒,醒酒﹑美容养颜的原料。
本发明方法通过酶碱组合控高分子果胶的酯化度和水解程度,酶水解和酒精纯化控制分 子量分布范围,获得了水溶性好,分子量分布范围窄,酯化度适中可控制的小分子果胶,制 得的小分子果胶适用于作为抑制肿瘤、降低放化疗毒副作用﹑降血糖血脂、提高免疫力、改 善胃肠道功能、解除重金属、解酒,醒酒﹑美容养颜的原料。
Claims (8)
1.一种酶碱结合生产小分子果胶的方法,其特征在于,包括如下步骤:
(1)先用果胶裂解酶将高分子果胶裂解至分子量至1500-50000Da的小分子果胶:
在浓度为3-12kg/100L、PH值为2.5-5.5的高分子果胶溶液中加入质量为高分子果胶粉干重0.05%-2.0%的果胶裂解酶,在20-50℃温度下水解0.5-10小时后冷却至室温获得分子量至1500-50000Da的小分子果胶。
(2)利用碱溶液对小分子果胶进行脱酯控制果胶的酯化度为2%-45%:
往步骤(1)水解得到的溶液加入碱性溶液,调节PH值至8-12进行脱酯,脱酯时间为0.25-10小时,用酸性溶液将溶液的pH调节至5.5-7.0,过滤去除不溶性固体得果胶透明溶液。
(3)往步骤(2)获得的透明果胶溶液中加入质量百分数为85%-95%酒精进行沉淀,然后过滤,滤渣用质量百分数为85-95%的酒精进行洗涤、离心脱水,干燥、粉碎、过80目筛后制得小分子果胶。
2.根据权利要求1所述的酶碱结合生产小分子果胶方法,其特征在于,所述的小分子果胶包括部分甲酯化的低聚半乳糖醛酸和半乳糖醛酸盐,包括钠、钾、钙、铁、锌和氨盐。
3.根据权利要求1所述的酶碱结合生产小分子果胶方法,其特征在于,获得的小分子果胶的分子量在1500-50000Da。
4.根据权利要求1所述的小分子果胶裂解酶碱结合的制备方法,其特征在于,所述高分子果胶溶液通过如下方法制备得到:
将高分子果胶粉搅拌下加入8-30倍无离子水中溶解,溶解温度20-50℃,溶液浓度3-12kg/100,得到高分子果胶溶液。
5.根据权利要求1所述的小分子果胶裂解酶碱结合的制备方法,其特征在于,将清洗干净的含果胶原料粉碎至20-150目,搅拌下加入含果胶原料重量15-50倍的无离子水中,加入硝酸调PH值至0.5-2.0,加温60-95℃提取果胶0.5-10小时,过滤除去残渣得果胶溶液;往果胶溶液中加入氨水或NaOH或碳酸钠中和至PH值2.5-5.5,果胶溶液冷却至20-50℃,精滤至溶液透明,再浓缩至浓度为3-12kg/100L,得到高分子果胶溶液。所述含果胶原料包括柑橘、柠檬、橙、桔、柚、苹果、等水果皮或果皮渣。
6.根据权利要求1所述的小分子果胶裂解酶碱结合的制备方法,其特征在于,将清洗干净的葵花盘粉碎至20-150目,搅拌下加入干葵花盘重量15-50倍的无离子水中,加入干葵花盘重量5%-15%草酸铵,加草酸调PH值至4.0-5.0,加温60-95℃提取果胶0.5-10小时,过滤除去残渣得果胶溶液;果胶溶液冷却至20-50℃,精滤至溶液透明,再浓缩至浓度为3-12kg/100L,得到高分子果胶溶液。
7.根据权利要求1-6任一项所述的酶碱结合生产小分子果胶方法,其特征在于,所述碱性溶液为氢氧化钠溶液或氢氧化钾溶液或氢氧化钠和氢氧化钾的混合溶液,酸性溶液为盐酸或硝酸溶液。
8.一种小分子果胶在制备食品、保健品、特殊医学配方食品、药品中的应用。
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