CN106880655B - 一种生产无农残食药提取物的方法 - Google Patents
一种生产无农残食药提取物的方法 Download PDFInfo
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- CN106880655B CN106880655B CN201710266554.XA CN201710266554A CN106880655B CN 106880655 B CN106880655 B CN 106880655B CN 201710266554 A CN201710266554 A CN 201710266554A CN 106880655 B CN106880655 B CN 106880655B
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- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
一种生产无农残食药提取物的方法,包括以下步骤:(1)将食材或药材切成薄片或粉碎,先置于弱极性有机溶剂中加热回流,过滤,脱溶剂,再置于水或乙醇水溶液中加热回流提取,过滤,冷却,得提取液;(2)将提取液过滤,透析,截留液浓缩,得浓缩液;(3)将浓缩液用先后串联的阳离子树脂和阴离子树脂吸附,收集流出液,再加水或乙醇水溶液将树脂柱内残留的料液赶出,收集水或醇赶液;(4)将流出液与水或醇赶液合并,浓缩,真空干燥,得无农残食药提取物。按照本发明方法所得食药提取物无农残检出;提取后所得目标有效成分的转移率≥85%;本发明方法适用范围广,生产连续性好,生产效率高、成本低,选择性吸附好,树脂可重复再生利用。
Description
技术领域
本发明涉及一种生产提取物的方法,具体涉及一种生产无农残食药提取物的方法。
背景技术
农残是农药使用后一定时期内没有被分解而残留于生物体、收获物、土壤、水体、大气中的微量农药原体、有毒代谢物、降解物和杂质的总称。导致和影响农药残留的原因有很多,其中农药本身的性质、环境因素以及农药的使用方法是影响农药残留的主要因素。施用于作物上的农药,其中一部分附着于作物上,一部分散落在土壤、大气和水等环境中,环境残存的农药中的一部分又会被植物吸收。残留农药直接通过植物果实或水、大气到达人、畜体内,或通过环境、食物链最终传递给人、畜。不慎食用了带有残留农药的食物,会出现的主要症状有:头晕、头疼、恶心、呕吐、倦乏、食欲减退、视力模糊、四肢发麻无力等;中毒较严重者,可能伴有腹痛、腹泻、出汗、肌肉颤动、精神恍惚、言语障碍、瞳孔缩小等症状;更严重者将出现昏迷痉挛、大小便失禁、瞳孔缩小如针尖、体温升高、呼吸麻痹等症状。
食材或药材的提取是对有效药用成分的富集,但同时也会富集农残等有害成分,高农残的食药提取物不仅不能起到良好的药用效果,甚至会危害人体健康,因此,脱除提取物中农残等有害成分非常必要。
CN104839378A公开了一种茶叶脱农残工艺,是通过原料拼配、低温水提、膜过滤、反渗透膜浓缩、树脂吸附、灭菌、喷雾干燥,得到脱农残速溶茶粉。但是,该方法仅使用大孔树脂吸附农残,对于农残含量较高、品种较多的产品,其选择性吸附较差,处理量小,树脂再生频繁,生产效率低、成本高。
CN102961422A公开了一种高纯度人参提取物的提取方法,是通过粉碎、醇提、铁钡复盐沉淀、大孔树脂吸附、筛分吸附树脂脱农残、浓缩干燥,得到高纯度无农残人参提取物。但是,该方法使用钡盐,存在安全隐患;且单用筛分树脂脱农残无法针对农残成分较多的情况。
CN103550273A公开了一种从人参中提取低农残人参皂苷的方法,是通过切断、冷提、浓缩、萃取、大孔树脂纯化,得到人参提取物。但是,由于该方法冷提时间过长,物料容易酸败,且提取效率低,没有明显的脱农残的工序。
CN101157731A公开了一种低农残人参、西洋参多糖提取物的制法,是通过醇提、水提、大孔树脂吸附制备无农残人参多糖。但是,该方法仅得到无农残多糖,人参皂苷未能制成脱农残提取物,原料利用不充分。
CN105315253A公开了一种黑米皮生产无农残黑米花青素的方法,是通过酶解水提、过滤、树脂吸附、树脂脱农残、干燥,得到无农残黑米皮花青素。但是,该脱农残的方法每批次处理量较少,且方法不具备弹性,当原料农残偏高或者种类变化时无法进行相应的调整。
CN106306991A公开了一种同时去除罗汉果提取物中农残和塑化剂的方法,是通过超临界提取、水溶、纳滤、干燥,得到脱塑化剂与农残的罗汉果提取物。但是,该方法农残和塑化剂脱除不够彻底。
发明内容
本发明所要解决的技术问题是,克服现有技术存在的上述缺陷,提供一种适用于多种含有高含量、种类复杂农残的食药原料,可提取水溶性或醇溶性有效成分,生产连续性好,处理量大、收率高,生产效率高、成本低,选择性吸附好,农残去除彻底,树脂可重复再生利用的生产无农残食药提取物的方法。
本发明解决其技术问题所采用的技术方案如下:一种生产无农残食药提取物的方法,包括以下步骤:
(1)提取:将食材或药材切成薄片或粉碎,先置于弱极性有机溶剂中加热回流,过滤,将滤渣干燥脱溶剂后,再置于水或乙醇水溶液中加热回流提取,过滤,冷却,得提取液;
(2)过滤、纳滤、浓缩:将步骤(1)所得提取液过滤,再将滤液透析,最后将透析所得截留液浓缩,得浓缩液;
(3)树脂吸附:将步骤(2)所得浓缩液用先后串联的阳离子树脂和阴离子树脂吸附,收集阴离子树脂柱流出液,上柱结束后,再通过在阳离子树脂和阴离子树脂柱中加水或乙醇水溶液,将树脂柱内残留的料液赶出至无有效成分检出,收集水或醇赶液;
(4)浓缩、干燥:将步骤(3)所得流出液与水或醇赶液合并,浓缩,真空干燥,得无农残食药提取物。
优选地,所述食材包括芹菜、大豆、山药、茶叶等中的一种或几种;所述药材包括罗汉果、人参、枸杞、菊花等中的一种或几种。
优选地,步骤(1)中,所述弱极性有机溶剂的总用量为食材或药材原料质量的8~20倍(更优选10~15倍)。若溶剂用量过少,则脱农残效果不佳,若溶剂用量过多,则溶剂回收量大,成本增加。
优选地,步骤(1)中,所述弱极性有机溶剂加热回流的温度为50~80℃,回流次数≥2次,每次回流的时间为1~3h。先用弱极性有机溶剂加热回流的目的是使原料中的农残进入回流液中,再通过过滤去除;在所述加热温度下,使得溶剂处于沸腾状态,更有利于溶剂与原材料的充分接触,去除农残效果更好。回流时间和次数可依据原材料的形态和农残的含量在所述范围内进行具体的调整。
优选地,步骤(1)中,所述弱极性有机溶剂为6#溶剂、正己烷、环己烷、二氯甲烷或乙酸乙酯等中的一种或几种。用弱极性有机溶剂加热回流的目的是去除农残,由于食材或药材的有效成分大多是水溶性或醇溶性的,所述弱极性溶剂可以脱除脂溶性农残,且不会损失有效成分。
优选地,步骤(1)中,所述干燥为鼓风干燥或真空干燥。
优选地,步骤(1)中,所述水或乙醇水溶液的总用量为食材或药材原料质量的15~40倍(更优选18~25倍)。
优选地,步骤(1)中,所述水或乙醇水溶液加热回流提取的温度为70~100℃(更优选85~95℃),回流次数≥2次,每次提取的时间为1~3h。
优选地,步骤(1)中,所述乙醇水溶液的体积浓度为30~70%(更优选55~65%)。
优选地,步骤(2)中,用陶瓷膜或超滤膜过滤,所述陶瓷膜或超滤膜的孔径为100~1000nm(更优选200~600nm)。用于除去提取液中不溶性的颗粒或悬浮物。
优选地,步骤(2)中,用纳滤膜进行透析,所述纳滤膜的孔径为100~30000Da(更优选200~10000Da,更进一步优选400~1000Da),透析的压力为1.8~2.5MPa。所述纳滤膜的孔径既要保证提取物中有效成分的截留,又要保证农残分子的透过。农残的分子量一般为300左右,比如,人参中人参皂苷的分子量为800左右,纳滤膜孔径适合选择500Da;罗汉果甜苷分子量为1200左右,纳滤膜孔径适合选择800Da。
优选地,步骤(2)中,所述透析的次数≥5次,每次透析至截留液量达到设备运转最小量时,加水或乙醇补足后再进行下次透析,透过纳滤膜的总液体体积(L)为食材或药材原料质量(kg)的30~50倍。增加透水量可降低截留液中的农残含量,最终可除去98%以上的农残,减少树脂所需吸附的农残量,有利于树脂再生利用,还可增加每批次产量,降低生产成本。
优选地,步骤(2)中,所述浓缩为真空浓缩,浓缩的温度为60~90℃(更优选75~85℃),真空度为-0.08~-0.1MPa,浓缩至料液固含量为3~7%。
优选地,步骤(3)中,树脂总体积与食材或药材原料质量的体积质量比(L/kg)为1:8~15。
优选地,步骤(3)中,所述浓缩液每小时的上柱流量为0.5~1.2倍(更优选0.8~1.0倍)树脂总体积。
优选地,步骤(3)中,用于赶出树脂柱内残留料液的水或乙醇水溶液的用量为2.5~5.0倍(更优选3~4倍)树脂总体积,流速与浓缩液上柱流速保持一致。
优选地,步骤(3)中,所述乙醇水溶液的体积浓度为30~70%(更优选55~65%)。
优选地,步骤(3)中,所述阳离子树脂和阴离子树脂的体积比为1:0.5~5.0(更优选1:0.6~2.0)。通过阳、阴离子串联使用,可增加树脂总量的高径比,提高农残吸附效果,适用于处理含有农残种类较复杂的产品,彻底脱除农残,制备无农残提取物。试验农残检验结果表明,阳、阴离子树脂的串联先后顺序不可逆。
优选地,步骤(3)中,所述阳离子树脂和阴离子树脂的装柱高径比均为4~7:1。
优选地,步骤(3)中,所述阳离子树脂为LX-N2、732或001*7,所述阴离子树脂为LX-N1、717或201*7。所述阴、阳离子树脂对目标提取物的有效成分无吸附,保证了有效成分的回收率;所述阴、阳离子树脂可用酸、碱再生,无需使用有机溶剂。
优选地,步骤(4)中,所述浓缩为真空浓缩,浓缩的温度为60~90℃(更优选75~85℃),真空度为-0.08~-0.1MPa,浓缩至料液固含量为40~60%(更优选45~55%)。
优选地,步骤(4)中,所述真空干燥的温度为60~90℃(更优选75~85℃),真空度为-0.08~-0.1MPa。
本发明方法的原理是:利用弱极性溶剂对脂溶性成分的良好溶解性,脱除原料中的脂溶性农残,利用农残和提取物有效成分的分子量之间的较大差异,通过纳滤膜的分子筛作用,除去产品中绝大部分水溶性农残和小分子杂质;再串联使用阳、阴离子树脂,采用吸附的方法,保证农残的彻底脱除。
本发明方法的有益效果如下:
(1)按照本发明方法所得食药提取物外检200项农残(欧盟标准),无农残检出;
(2)本发明方法可提取多种水溶性或醇溶性有效成分,提取后所得目标有效成分的转移率≥85%;
(3)本发明方法适用于多种含有高含量、种类复杂农残的食药原料的提取物制备,生产连续性好,处理量大,生产效率高、成本低,选择性吸附好,树脂可重复再生利用。
具体实施方式
下面结合实施例对本发明作进一步说明。
本发明实施例所使用的人参为市售东北人参根原料,总皂苷的质量含量为1.06%,其中,Rg1 0.24%、Re 0.47%、Rb1 0.35%,原料农残的质量含量为1.83ppm,其中,五氯苯胺0.21ppm,腐霉利0.33ppm,三唑醇0.15ppm,稻瘟灵0.29ppm,戊唑醇0.15ppm,多菌灵0.25ppm,烯酰吗啉0.45ppm;
本发明实施例所使用的罗汉果购于广西桂林,罗汉果甜苷V的质量含量为1.24%,原料农残的质量含量为0.14ppm,其中,烯酰吗啉0.05ppm,腈菌唑0.04ppm,氟环唑0.02ppm,恶霜灵0.03ppm;
本发明实施例所使用的茶叶购于湖南安化,EGCG的质量含量为8.55%,原料农残的质量含量为0.11ppm,其中,六六六0.03ppm,戊唑醇0.02ppm,烯酰吗啉0.04ppm,苯醚甲环唑0.02ppm;
本发明实施例所使用的LX-N2阳离子树脂和LX-N1阴离子树脂均购于蓝晓科技;
本发明实施例所使用的原料、化学试剂,如无特殊说明,均通过常规商业途径获得。
实施例1
(1)提取:将500kg人参原料切成薄片,先置于6#溶剂中,在60℃下,加热回流3次,每次6#溶剂的用量分别为2000L、1500L、1500L,时间均为1h,过滤,将滤渣经鼓风干燥脱溶剂后,再置于体积浓度60%的乙醇水溶液中,在90℃下,加热回流提取4次,每次乙醇水溶液的用量分别为3000L、2000L、2000L、2000L,提取时间分别为2h、1h、1h、1h,过滤,冷却,合并得提取液;
(2)过滤、纳滤、浓缩:将步骤(1)所得提取液用孔径200nm的陶瓷膜过滤,再将滤液用孔径500Da的纳滤膜透析,透析的压力为2MPa,共透析8次,每次透析至截留液量达到设备运转最小量时,加入乙醇2000L补足后再进行下次透析,总透过量为24000L,将透析所得截留液在80℃,真空度-0.09MPa下,真空浓缩至固含量为5.5%,得浓缩液;
(3)树脂吸附:将步骤(2)所得浓缩液,用先后串联的LX-N2阳离子树脂和LX-N1阴离子树脂吸附,阳离子树脂与阴离子树脂的体积各为25L,阳离子树脂与阴离子树脂装柱的高径比均为4:1,浓缩液的上柱流速为50L/h,收集阴离子树脂柱流出液,上柱结束后,再通过在阳离子树脂和阴离子树脂柱中加入150L体积浓度为60%的乙醇水溶液,在上柱流速为50L/h下,将树脂柱内残留的料液赶出至无皂苷检出,收集醇赶液;
(4)浓缩、干燥:将步骤(3)所得流出液和醇赶液合并,在80℃,真空度-0.09MPa下,真空浓缩至料液固含量为53%,再在80℃,真空度-0.1MPa下真空干燥,即得17.8kg无农残人参提取物。
经HPLC检测,所得无农残人参提取物中,总皂苷质量含量为25.68%,其中,Rg15.8%、Re 11.3%、Rb1 8.57%,总皂苷转移率为86.2%;外检200项农残(欧盟标准)结果表明:无农残检出。
实施例2
(1)提取:将800kg罗汉果粉碎,先置于乙酸乙酯中,在80℃下,加热回流2次,每次乙酸乙酯的用量分别为4800L、4000L,时间分别为2h、1h,过滤,将滤渣经鼓风干燥脱溶剂后,再置于纯水中,在95℃下,加热回流3次,每次纯水的用量分别为6400L、5600L、4800L,提取时间分别为2h、1h、1h,过滤,冷却,合并得提取液;
(2)过滤、纳滤、浓缩:将步骤(1)所得提取液用孔径500nm的陶瓷膜过滤,再将滤液用孔径800Da的纳滤膜透析,透析的压力为2MPa,共透析6次,每次透析至截留液量达到设备运转最小量时,加入纯水2000L补足后再进行下次透析,总透过量为28000L,将透析所得截留液在80℃,真空度-0.09MPa下,真空浓缩至固含量为6.1%,得浓缩液;
(3)树脂吸附:将步骤(2)所得浓缩液,用先后串联的LX-N2阳离子树脂和LX-N1阴离子树脂吸附,阳离子树脂与阴离子树脂的体积分别为40L、25L,阳离子树脂与阴离子树脂装柱的高径比分别为6:1、4:1,浓缩液的上柱流速为60L/h,收集阴离子树脂柱流出液,上柱结束后,再通过在阳离子树脂和阴离子树脂柱中加入200L纯水,在上柱流速为60L/h下,将树脂柱内残留的料液赶出至无甜苷检出,收集水赶液;
(4)浓缩、干燥:将步骤(3)所得流出液和水赶液合并,在80℃,真空度-0.09MPa下,真空浓缩至料液固含量为55%,再在80℃,真空度-0.1MPa下真空干燥,即得21.8kg无农残罗汉果提取物。
经HPLC检测,所得无农残罗汉果提取物中,甜苷V的质量含量为41.3%,转移率为90.8%;外检200项农残(欧盟标准)结果表明:无农残检出。
实施例3
(1)提取:将800kg茶叶粉碎,先置于二氯甲烷中,在50℃下,加热回流3次,每次二氯甲烷的用量分别为4800L、4000L、3200L,时间分别为2h、1h、1h,过滤,将滤渣经真空干燥脱溶剂后,再置于纯水中,在95℃下,加热回流3次,每次纯水的用量分别为5600L、4800L、4000L,提取时间每次均为1h,过滤,冷却,合并得提取液;
(2)过滤、纳滤、浓缩:将步骤(1)所得提取液用孔径200nm的超滤膜过滤,再将滤液用孔径400Da的纳滤膜透析,透析的压力为2MPa,共透析6次,每次透析至截留液量达到设备运转最小量时,加入纯水2000 L补足后再进行下次透析,总透过量25000L,将透析所得截留液在80℃,真空度-0.09MPa下,真空浓缩至固含量为5.1%,得浓缩液;
(3)树脂吸附:将步骤(2)所得浓缩液,用先后串联的LX-N2阳离子树脂和LX-N1阴离子树脂吸附,阳离子树脂与阴离子树脂的体积分别为25L、30L,阳离子树脂与阴离子树脂装柱的高径比分别为4:1、5:1,浓缩液上柱流速为50L/h,收集阴离子树脂柱流出液,上柱结束后,再通过在阳离子树脂和阴离子树脂柱中加入200L纯水,在上柱流速为50L/h下,将树脂柱内残留的料液赶出至无EGCG检出,收集水赶液;
(4)浓缩、干燥:将步骤(3)所得流出液和水赶液合并,在80℃,真空度为-0.09MPa下,真空浓缩至料液固含量为51%,再在80℃,真空度-0.1MPa下真空干燥,即得95.5kg无农残茶叶提取物。
经HPLC检测,所得无农残茶叶提取物中,EGCG的质量含量为63.8%,转移率为89.1%;外检200项农残(欧盟标准)结果表明:无农残检出。
Claims (9)
1.一种生产无农残食药提取物的方法,其特征在于,包括以下步骤:
(1)提取:将食材或药材切成薄片或粉碎,先置于弱极性有机溶剂中加热回流,过滤,将滤渣干燥脱溶剂后,再置于水或乙醇水溶液中加热回流提取,过滤,冷却,得提取液;所述弱极性有机溶剂为6#溶剂、正己烷、环己烷、二氯甲烷或乙酸乙酯中的一种或几种;所述食材为茶叶,所述药材为罗汉果或人参;
(2)过滤、透析、浓缩:将步骤(1)所得提取液过滤,再将滤液透析,最后将透析所得截留液浓缩,得浓缩液;所述过滤用陶瓷膜或超滤膜过滤,所述陶瓷膜或超滤膜的孔径为100~1000nm;所述透析用纳滤膜进行透析,所述纳滤膜的孔径为100~30000Da,透析的压力为1.8~2.5MPa;
(3)树脂吸附:将步骤(2)所得浓缩液用先后串联的阳离子树脂和阴离子树脂吸附,收集阴离子树脂柱流出液,上柱结束后,再通过在阳离子树脂和阴离子树脂柱中加水或乙醇水溶液,将树脂柱内残留的料液赶出至无有效成分检出,收集水或醇赶液;所述阳离子树脂为LX-N2、732或001*7,所述阴离子树脂为LX-N1、717或201*7;
(4)浓缩、干燥:将步骤(3)所得流出液与水或醇赶液合并,浓缩,真空干燥,得无农残食药提取物。
2.根据权利要求1所述生产无农残食药提取物的方法,其特征在于:所述弱极性有机溶剂为6#溶剂、二氯甲烷或乙酸乙酯。
3.根据权利要求1或2所述生产无农残食药提取物的方法,其特征在于:步骤(1)中,所述弱极性有机溶剂的总用量为食材或药材原料质量的8~20倍;所述弱极性有机溶剂加热回流的温度为50~80℃,回流次数≥2次,每次回流的时间为1~3h。
4.根据权利要求1或2所述生产无农残食药提取物的方法,其特征在于:步骤(1)中,所述水或乙醇水溶液的总用量为食材或药材原料质量的15~40倍;所述水或乙醇水溶液加热回流提取的温度为70~100℃,回流次数≥2次,每次提取的时间为1~3h;所述乙醇水溶液的体积浓度为30~70%。
5.根据权利要求1或2所述生产无农残食药提取物的方法,其特征在于:步骤(2)中,所述透析的次数≥5次,每次透析至截留液量达到设备运转最小量时,加水或乙醇补足后再进行下次透析,透过纳滤膜的总液体体积为食材或药材原料质量的30~50倍,所述总液体体积的单位为L,所述食材或药材原料质量的单位为kg。
6.根据权利要求1或2所述生产无农残食药提取物的方法,其特征在于:步骤(2)中,所述浓缩为真空浓缩,浓缩的温度为60~90℃,真空度为-0.08~-0.1MPa,浓缩至料液固含量为3~7%。
7.根据权利要求1或2所述生产无农残食药提取物的方法,其特征在于:步骤(3)中,树脂总体积与食材或药材原料质量的体积质量比为1:8~15;所述浓缩液每小时的上柱流量为0.5~1.2倍树脂总体积;用于赶出树脂柱内残留料液的水或乙醇水溶液的用量为2.5~5.0倍树脂总体积,流速与浓缩液上柱流速保持一致;所述乙醇水溶液的体积浓度为30~70%。
8.根据权利要求1或2所述生产无农残食药提取物的方法,其特征在于:步骤(3)中,所述阳离子树脂和阴离子树脂的体积比为1:0.5~5.0;所述阳离子树脂和阴离子树脂的装柱高径比均为4~7:1。
9.根据权利要求1或2所述生产无农残食药提取物的方法,其特征在于:步骤(4)中,所述浓缩为真空浓缩,浓缩的温度为60~90℃,真空度为-0.08~-0.1MPa,浓缩至料液固含量为40~60%;所述真空干燥的温度为60~90℃,真空度为-0.08~-0.1MPa。
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