CN113143994B - 肉桂油生产残渣水提物及其用途 - Google Patents
肉桂油生产残渣水提物及其用途 Download PDFInfo
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- CN113143994B CN113143994B CN202110023246.0A CN202110023246A CN113143994B CN 113143994 B CN113143994 B CN 113143994B CN 202110023246 A CN202110023246 A CN 202110023246A CN 113143994 B CN113143994 B CN 113143994B
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- cinnamon oil
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Images
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- A—HUMAN NECESSITIES
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- A23K10/30—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms
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Abstract
本发明提供了一种肉桂枝叶挥发油提取残渣的提取方法，包括以下步骤：肉桂枝叶残渣加水，热回流提取或常压煎煮，提取液过滤后经浓缩、冷冻干燥得到废渣水提物的冻干粉，即得。还提供了上述提取物在制备抑制黄曲霉的药物、功能性食用菌培养基、畜禽饲料、有机肥中的应用。
Description
技术领域
本申请涉及医药环保领域，尤其涉及肉桂油生产残渣水提物及其用途。
背景技术
肉桂精油广泛用于食品、日用品、功能性材料等领域，通常为樟科植物肉桂的干燥枝、叶经水蒸气蒸馏法提取得到的。我国肉桂油的年产量已超过85万公斤，而精油只占肉桂枝叶干重的1.0％左右，约84000 吨的提取残渣被直接焚烧和丢弃，这不仅造成了资源的浪费，对环境也构成了潜在隐患，对残渣的处理和再利用是一个重要的值得关注的方向。
目前的研究表明，肉桂油提取后的残渣中含有大量的次生代谢产物，包括糖类、有机酸、黄酮(苷) 类、萜(苷)类、多酚类、苯丙素类等，这些化合物具有多种生物活性，在抗菌、抗炎、抗氧化、降血糖等多个方面具有显著效果。
黄曲霉毒素(AFT)是黄曲霉和寄生曲霉等某些菌株产生的双呋喃环类毒素，其衍生物有约20种，分别命名为B1、B2、G1、G2、M1、M2等，其中B1的毒性最大，是砒霜的68倍。1993年，黄曲霉毒素被世界卫生组织(WHO)癌症研究机构划定为1类致癌物，其危害在于对人体及动物肝脏组织有破坏作用，诱发恶性肝细胞癌。黄曲霉毒素及其产生菌在自然界中分布广泛，易侵染玉米、花生、坚果等粮油经济作物，严重威胁我国食品安全和农产品出口贸易。因此，研发绿色安全高效的黄曲霉毒素抑制剂一直是研究的热点。
经检索，目前对于肉桂油提取后的残渣重复利用的研究并不多见。其中，CN111423285A涉及一种肉桂枝叶基质生物肥料的制备方法；CN106350214A公开了从肉桂枝和/或肉桂叶提取肉桂油的水蒸气循环蒸馏方法及蒸后废渣的资源化利用，以从废渣中继续提取肉桂油；CN105010337A提供了一种利用肉桂油提取废液制备蚊子驱避剂的方法；CN105124716A公开了一种利用肉桂油提取废液制备食品防腐剂的方法，涉及一种制备食品防腐剂的方法，本发明利用从肉桂油提取器的油水分离器中流出的水相馏出液或是将提取器中的棕黑色浑浊废液重新蒸馏后收集的水相馏出液，通过加入氯化钠或氯化钾，使水相馏出液中的反式-肉桂醛和肉桂酸析出，再加入有机溶剂进行萃取，然后对有机溶剂进行减压蒸馏，得到棕色油状液体，将此棕色油状液体低温冷冻，析出结晶，快速过滤即得到反式-肉桂醛和肉桂酸混合物。反式-肉桂醛和肉桂酸混合物对金黄色葡萄球菌、大肠杆菌、枯草杆菌、黑曲霉、黄曲霉和桔青霉具有抑菌活性，对DPPH·自由基具有清除作用，可作为食品防腐剂。此外，《发酵桂叶渣挥发性芳香气体成分固相微萃取气相色谱-质谱联用分析研究》采用顶空固相微萃取气质联用的方法分析发酵桂叶渣的挥发性香味成分,固相微萃取的条件为:萃取时间10min,萃取温度90℃,色谱分离得到106种挥发性成分,66种可被鉴定,其主成分为乙酸乙酯(8.375％)、己酸丁酯(6.337％)、丁酸丁酯(4.866％)、δ-荜澄茄烯(4.612％)、r-衣兰油烯(4.405％)、α- 衣兰油烯(3.416％)、古巴烯(3.313％)等；《紫外分光光度法检测桂叶、桂叶渣总黄酮研究》采用紫外分光光度计法检测桂叶及桂叶渣提取液黄酮浓度。结果表明，桂叶及桂叶渣提取液黄酮浓度分别为2.56,1.18 g/L,精密度RSD分别为0.308％,1.13％,重复性RSD分别为1.07％,3.82％。《肉桂渣开发饲料添加剂研究前景》利用肉桂渣研究开发一种生物饲料及饲料添加剂将具有广阔的前景。
综上，目前对于肉桂油提取后残渣重复利用的研究主要集中在对其化学成分的研究、蚊子驱避剂、饲料/肥料应用和防腐剂的应用上。其中，虽然CN105124716A公开了残渣中的反式-肉桂醛和肉桂酸混合物对金黄色葡萄球菌、大肠杆菌、枯草杆菌、黑曲霉、黄曲霉和桔青霉具有抑菌活性，但是其对残渣成分的分析不够全面，按照其制备方法获得的产品仍然存在利用不够充分，抑菌效果不够显著的缺点。
本研究对肉桂油产业中的提取残渣进行了提取分离，研究其对黄曲霉生长及产毒的抑制作用，筛选出 50％乙醇洗脱部位是抑制效果最好的富集部位。并采用液质联用对其活性成分进行分析，结果显示，黄酮苷类、萜苷类是其主要的成分。进一步的，我们选择了其中具有突出的抑制作用的成分进行研究，发现了成分之间的协同抑制作用。该发现尚未见相关报道，表明肉桂油生产残渣可作为一种易得廉价的黄曲霉毒素抑制剂的原料来源，为肉桂油生产残渣在功能性食用菌培养基、畜禽饲料、有机肥的开发上提供了依据。
发明内容
本发明提供了一种肉桂油生产残渣水提物的提取方法，包括以下步骤：肉桂枝叶残渣加水，热回流提取或常压煎煮，提取液过滤后经浓缩、干燥后即得冻干粉。
其中，所述的肉桂枝叶残渣是肉桂枝叶提取挥发油后剩余的部分。
所述的干燥优选冷冻干燥。
进一步的，所述的水用量为药材的8-12倍，优选10倍；
进一步的，热回流加热温度为100-500℃，优选350℃；
进一步的，热回流或煎煮时间为1-3h，优选2h；
本发明还进一步提供上述冻干粉的提取方法，包括以下步骤：将冻干粉采用大孔树脂梯度洗脱，溶剂分别为：水、30％乙醇、50％乙醇、70％乙醇和95％乙醇，得到相应洗脱部位，浓缩后冷冻干燥即得。
进一步的，所述的大孔树脂为AB-8型大孔树脂。
进一步的，优选50％乙醇得到的相应洗脱部位，浓缩后冷冻干燥得到的提取物。
本发明还提供上述肉桂枝叶挥发油残渣的提取方法所获得的提取物。
进一步的，所述提取物含有下述化合物：cinnzeylanine(瑞诺烷型二萜类)、cinnzeylanol(瑞诺烷型二萜类)、ciwujiatone(木脂素类)。
本发明的提取物进一步含有：lyoniresinol 3-O-D-glucopyranoside(木脂素类)、cinncassins A4 (内酯类)、kaempferol 3-O-vicianoside(黄酮类)。
进一步的，本发明提取物中所述化合物的重量比为Cinnzeylanine 8-12：cinnzeylanol 4-8： ciwujiatone 4-8：lyoniresinol 3-O-D-glucopyranoside 6-10：cinncassins A4 6-10：kaempferol 3-O-vicianoside 6-10。
进一步的，本发明提取物中所述化合物的重量比为cinnzeylanine 10：cinnzeylanol 6：ciwujiatone 6：lyoniresinol 3-O-D-glucopyranoside 8：cinncassinsA4 8：kaempferol 3-O-vicianoside 8。
本发明还提供一种组合物，其含有下述化合物：Cinnzeylanine(瑞诺烷型二萜类)、cinnzeylanol(瑞诺烷型二萜类)、ciwujiatone(木脂素类)。
本发明的组合物进一步含有：lyoniresinol 3-O-D-glucopyranoside(木脂素类)、cinncassins A4 (内酯类)、kaempferol 3-O-vicianoside(黄酮类)。
进一步的，本发明组合物中所述化合物的重量比为Cinnzeylanine 8-12：cinnzeylanol 4-8： ciwujiatone 4-8：lyoniresinol 3-O-D-glucopyranoside 6-10：cinncassins A4 6-10：kaempferol 3-O-vicianoside 6-10。
进一步的，本发明组合物中所述化合物的重量比为Cinnzeylanine 10：cinnzeylanol 6：ciwujiatone 6：lyoniresinol 3-O-D-glucopyranoside 8：cinncassinsA4 8：kaempferol 3-O-vicianoside 8。
本发明还提供上述提取物或组合物在制备抑制黄曲霉的药物、功能性食用菌培养基、畜禽饲料、有机肥中的应用。
进一步的，本发明所述的化合物结构如下：
附图说明
图1 1mg/mL浓度下的抑菌效果图注：T2旁边的不是杂菌，是加孢子液时滴在旁边的菌液
图2 5mg/mL浓度下的抑菌效果图
图3 10mg/mL浓度下的抑菌效果图
图4 4种毒素的MRM色谱图(定量离子)
图5 T2 1mg/mL处理下4种毒素的MRM色谱图(定量离子)
具体实施方式
实施例1
1实验材料
1.1样品:肉桂枝叶提取残渣加10倍水，350℃加热条件下回流提取2h，提取液过滤后，经浓缩冷冻干燥得废渣水提物的冻干粉，编号T1，-20℃保存。将AB-8大孔树脂填充进内径5cm的玻璃柱，装成填料高26cm的大孔树脂柱。部分冻干粉T1(8.3g)溶解后上样，梯度洗脱溶剂为：水、30％乙醇、50％乙醇、 70％乙醇和95％乙醇，得到相应洗脱部位，分别编号为T2、T3、T4、T5、T6，浓缩后冷冻干燥以冻干粉形式储存。各部位的洗脱体积和产率如下表所示：
Table 1洗脱程序
1.2试剂：马铃薯葡萄糖琼脂培养基(PDA)(马铃薯浸粉6g，葡萄糖20g，琼脂20g)，为Solarbio 公司产品；黄曲霉毒素AFB1、AFB2、AFG1和AFG2对照品购自普瑞邦公司，纯度>98.0％；MFC100小柱购自普瑞邦公司。
1.3仪器：Waters UPLC-QqQ-MS/MS液质联用仪；SW-CJ-2D型双人净化工作台，上海苏净实业有限公司；RXZ-158A型智能人工气候箱，宁波江南仪器厂；DHG-9245A型电热鼓风干燥箱，上海一恒科学仪器有限公司；ZEALWAY GR60DA型立式自动压力蒸汽灭菌器，致微(厦门)仪器有限公司；PL203型千分之一电子天平，梅特勒-托利多仪器(上海)有限公司；Dlamond TⅡ型纯水仪，Thermo Fisher Scientific。
1.4菌株:黄曲霉(Aspergillus flavus,CGMCC 3.4410)，北京协和医学院中国医学科学院药用植物研究所分析化学实验室提供。
2实验方法
2.1菌种活化及孢子悬浮液制备
将甘油保藏的黄曲霉菌株接种到PDA培养基上，28℃下培养7d进行活化。取一个已培养好的菌株平板，加入无菌水(121℃,30min)10mL，用无菌接种环将琼脂表面的孢子轻轻刮下，吸取悬浮液于已灭菌的50ml离心管中，涡旋振荡制成均匀的孢子悬浮液，血球计数板计数，将孢子浓度稀释到1×107个 /mL。
2.2抑菌效果测定
将T1-T6用无菌水溶解，超声溶解，加入培养基中，使最终浓度分别为1mg/mL,5mg/mL，和10mg/mL，以未添加肉桂提取物的PDA培养基作为对照，倒入培养皿中，静置凝固，每个处理3个重复。吸取2μL 黄曲霉孢子悬浮液接种于PDA平板中央至完全吸收。用保鲜膜密封，放置于28℃培养箱中培养7d。
2.3黄曲霉毒素的测定
2.3.1仪器方法色谱柱：BEH C18(100mm×2.1mm i.d.,1.7μm,Waters Corp.)，柱温：35 ℃；流动相：0.2mM乙酸铵水溶液(A)-甲醇(B，含-0.1％甲酸)，梯度洗脱：0min:25％A；4min:45％A； 10min:90％A；12min:90％A；12.1min:25％，流速0.3mL/min，进样量2μL。
质谱条件：ESI离子源，正离子模式，MRM检测；毛细管电压3.5kV，离子源温度150℃，去溶剂温度350℃，黄曲霉毒素的质谱条件见下表：
Table 2四种毒素的MS参数
“*”定量离子
2.3.2前处理方法将培养皿放置于生物安全柜中，灭菌，于60℃下烘干至恒重，转移至50mL的离心管中，加入80％的乙腈50mL超声45min，过滤，取滤液5mL，过MFC 100小柱，取滤液1ML用80％的乙腈稀释10倍，取适量过0.22μm微孔滤膜，UPLC-MS/MS检测。
2.3.3对照品溶液的配置精密吸取4种毒素对照品的溶液适量，置于5mL的容量瓶中，用甲醇水 (80:20,v/v)配置为一定浓度的混标(AFB1,200ng/mL，AFB2,100ng/mL,AFG1,100ng/mL，AFG2, 50ng/mL)，4℃保存。取混合对照品的储备液，用空白基质溶液配置成浓度在0.1～100ng/mL之间的标准工作液，至少6个浓度。
2.3.4标准曲线的测定在上述的UPLC-MS/MS条件下进样，以定量离子的峰面积为纵坐标，以对照品的浓度为横坐标进行回归分析，分别绘制4种真菌毒素的标准曲线。得到相应的回归方程、相关系数、线性范围，并测定其定量限、精密度，具体结果如下：
Table 3四种真菌毒素对照品的回归方程、定量限、精密度
3实验结果
3.1在上述三个浓度下各提取的抑菌效果图见说明书附图1-3，抑菌直径如下：
Table 4 1mg/mL浓度下菌落平均直径
Table 5 5mg/mL浓度下菌落平均直径
Table 6 10mg/mL浓度下菌落平均直径
【注：5mg/mL和10mg/mL为同一批次，使用的为同一对照；培养基中加入提取物后有颜色的变化；通过SPSS软件进行显著性差异分析，不同字母之间表示有显著性差异(P＜0.05,n＝3)】
按照以下公式计算抑菌率：抑菌率(％)＝(dc-dt)/dc*100％，式中：dc为对照组中菌丝平均直径(mm)；dt为实验组中菌丝平均直径(mm)。
由表可知：①提高供试浓度后(1→5mg/mL)，废渣水提物(T1)显示出了抑制菌落生长的作用。
②提高供试浓度后(1→5mg/mL)，废渣水提物的70％乙醇洗脱物(T5)、95％乙醇洗脱物(T6)显示出抑制菌落生长的作用，随着浓度的继续增加(5→10mg/mL)，抑制作用随之增强。
3.2黄曲霉毒素含量测定结果
不同处理中真菌毒素的含量如下：
Table 7 1mg/mL处理下毒素含量(μg,n＝3)
“-”未检测到
Table 8 5mg/mL处理下毒素含量(μg,n＝3)
“-”未检测到
Table 9 10mg/mL处理下毒素含量(μg,n＝3)
基于上述各提取物对黄曲霉菌生长的影响作用结果，进一步研究了其对黄曲霉菌产毒力的作用。AFB1、 AFB2、AFG1、AFG2是黄曲霉菌的主要代谢产物，其中，AFB1最常见、毒性最强。
由上表可知，①废渣水提物(T1)在未显示出抑制菌落生长的情况下，表现出了显著的抑制毒素分泌的作用，而且随着浓度提高，抑制力增强。
②供试浓度梯度下，50％乙醇洗脱物(T4)在能促进菌落生长的情况下，均表现出了显著的抑制毒素分泌的作用。
③在能抑制菌落生长的情况下，70％乙醇洗脱物(T5)、95％乙醇洗脱物(T6)组在高浓度下，抑制了毒素的分泌。
综合以上结果，废渣水提物具有抑制黄曲霉菌产AFB1毒素的作用，抑制率可达83.5％。经过富集后， 50％，70％，95％乙醇洗脱部位表现出较强的抑制黄曲霉菌产毒的作用，而50％乙醇洗脱部位的产率最高，为 24.6％，因此选择50％乙醇洗脱部位进行后续的开发研究。5mg/mL浓度下，50％乙醇洗脱部位的抑制率高达90.7％，10mg/mL下，抑制率达到100％，这一结果为高效，绿色的黄曲霉毒素抑制剂的开发提供了依据。
实施例2
通过对抑菌效果最好的50％乙醇洗脱物(T4)的成分进行分析，其主要含有下述化合物：Cinnzeylanine (瑞诺烷型二萜类)、cinnzeylanol(瑞诺烷型二萜类)、ciwujiatone(木脂素类)、lyoniresinol 3-O-D-glucopyranoside(木脂素类)、cinncassins A4(内酯类)、kaempferol 3-O-vicianoside(黄酮类)；其重量比约为10：6：6：8：8：8(模拟在T4中的成分比例)。
在此基础上，本研究进一步采用上述比例的化合物进行实验，发现该采用该配比的组合物，在其浓度为0.01mg/mL，0.02mg/mL，0.05mg/mL，0.1mg/mL，0.2mg/mL时，均未能检测到黄曲霉毒素，获得了优异的抑制毒素效果。相关实验方法与实施例1相同，结果见下表。
Table 10黄曲霉毒素含量(μg,n＝3)
“-”未检测到
近年来以中药废渣为原料制备食用菌培养基、畜禽饲料、有机肥等方面的研究取得了一些成效，本研究证明了肉桂提取废渣对黄曲霉菌生长和产毒有抑制作用，可为预防黄曲霉毒素的功能性食用菌培养基、畜禽饲料、有机肥的开发提供依据。
Claims (2)
1.一种组合物，其含有下述化合物：c innzeylanine、cinnzeylanol、ciwujiatone、lyoniresinol 3-O-D-glucopyranoside、cinncassins A4、kaempferol 3-O-vicianoside，其重量比为10:6:6:8:8:8；所述的化合物结构如下：
2.权利要求 1所述的组合物在制备抑制黄曲霉的药物、功能性食用菌培养基、畜禽饲料和有机肥中的应用。
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