CN114053162A - 一种颜色稳定的含山梨酸的防腐剂组合物及应用 - Google Patents
一种颜色稳定的含山梨酸的防腐剂组合物及应用 Download PDFInfo
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Abstract
本发明公开了一种颜色稳定的含山梨酸的防腐剂组合物及应用。本防腐剂组合物由占组合物总重量5~35%的有机酸、0.05~2%的稳定剂、10~40%的增溶剂、1~20%的协同增效剂及20~80%的溶剂组成。本组合物克服了山梨酸易变色及水溶性差的缺陷,通过组分间的协同作用,使含山梨酸的组合物在高温、光照、接触氧气条件下均能保持颜色稳定,且水溶性佳,并有较好的防腐效果,可广泛应用于化妆品、家居洗涤用品、湿巾等产品中。
Description
技术领域
本发明涉及一种颜色稳定的含山梨酸的防腐剂组合物及应用,尤其是涉及含山梨酸的水溶性佳,在高温、光照、接触氧气条件下均能保持颜色稳定的防腐剂组合物及应用。
背景技术
山梨酸的化学名称为2,4一己二烯酸,结构式为CH3CH=CHCH=CHCOOH。纯山梨酸是一种无色针状结晶或白色结晶性粉末,无臭或略有特殊气味。熔点132~135℃,沸点228℃(分解温度)。纯品在密封状态下较稳定,在空气中放置易被氧化着色。易溶于醇、醚等有机溶剂,微溶于水。在水中的溶解度(g/100g),20℃时为0.16,100℃也只有3.8,因而在水性配方中不易添加使用。
山梨酸及山梨酸钾是***粮农组织和世界卫生组织推荐的国际公认、广谱、高效、安全的食品防腐保鲜剂。山梨酸及其盐类也是世界各国允许使用的化妆品防腐剂,同时作为抑菌剂品种还被各国药典收录。山梨酸的分子结构中含有羧基和共轭双键,羧基使山梨酸呈酸性,抑制微生物的生长;共轭双键可与微生物酶的巯基结合(pH<6的情况下),从而破坏酶系结构,使酶失去活性,最终抑制微生物繁殖,达到防腐保鲜目的。山梨酸需要通过细胞膜才可抑制酶***,未离解的山梨酸分子才能起作用。在酸性条件(pH<6)下,山梨酸对霉菌、酵母菌和需氧菌均有抑制作用,但对厌氧芽孢形成菌与嗜酸乳杆菌几乎无效。近年的研究表明,山梨酸比同碳数饱和羧酸具有较高的抗菌活性,也能防止肉毒杆菌、金黄色葡萄球菌、沙门杆菌等的生长。不饱和脂肪酸是饱和脂肪酸同化作用的中间产物,在体内可正常地参加新陈代谢,并被同化产生二氧化碳和水,故山梨酸可被视成是食品的成分,对人体是无害的。
目前,山梨酸及其盐已广泛应用于食品、饮料、酱菜、罐头、烟草、医药、化妆品、农产品、饲料等行业。在化妆品及个人护理品中,中国、欧盟皆规定其最大允许使用浓度为0.6%(以酸计);日本规定最大使用浓度为0.5%(总量);美国CIR则给出使用浓度山梨酸不超过5%、山梨酸钾不超过1%是安全的评价结论。
山梨酸微溶于水,不易添加使用。山梨酸的盐类溶于醇、二醇,极易溶于水,如山梨酸钾20℃时在水中的溶解度为138g/100g。山梨酸盐易于添加,但仍需在酸性条件(pH<6)下,转化为非离解的山梨酸分子发挥抗菌作用,使得配方中添加的山梨酸盐因形成山梨酸分子同样具有沉淀析出的风险。由于分子结构的特点,山梨酸及其盐类都易被氧化导致变色,特别是在溶液配方中变色更是明显。易变色的特点不仅会影响产品特别是化妆品的外观,严重的还会影响产品的气味、风味及抗菌效果。
在现有技术中,为了防止山梨酸及其盐发生变色,通常添加一些金属离子、尿囊素、络合剂或抗氧化剂等以达到一定效果。
中国专利公开号CN1175899A,发明名称为“抑制食品和化妆组合物中由山梨酸盐导致的棕色变色的方法”,公开了一种在视觉和感觉上稳定用山梨酸盐防腐的食品和化妆品组合物的方法,通过利用尿囊素或尿囊素和柠檬酸盐作为棕色变色抑制剂达到发明效果,尿囊素与柠檬酸盐具有协同作用,在水溶液中的山梨酸盐6个月内颜色变化较小,但没有涉及保质期较长的化妆品(一般2~3年)长期颜色稳定情况,也没有涉及解决山梨酸在水溶液中的溶解性差的问题。
美国专利公开号US966246,发明名称“稳定的山梨酸或其盐”,通过加入金属离子(例如:锰、铜、锌和钴等)来降低由山梨酸盐导致的棕色变色和气味变化。但由于生理上的不可接受,在食品和化妆品中加入这些重金属离子来稳定颜色一般也是不恰当、不适用的。
此外,还有有文献[Domsch,A.(1994):Die Kosmetischen Praparate,Volume 2;Wassrige und tensidhaltige Formulierungen,4th edition,page 329,Augsburg;Verlgfur die chemische Industrie]报道,在相对长时间储存的化妆品中受到氧化的影响,山梨酸盐仍然出现变色问题。迄今为止最常采用的保护措施是使用络合剂(EDTA或柠檬酸盐),可以延缓山梨酸盐导致的颜色变化。然而,在透明的塑料瓶中,仍然存在上述变色问题,尤其是在高温情况下。说明加入络合剂防止变色的方法,依然受限于使用包装及使用环境。
发明内容
本发明提供一种颜色稳定的含山梨酸的防腐剂组合物,克服了山梨酸易变色及水溶性差的缺陷,通过组分间的协同作用,使含山梨酸的组合物在高温、光照、接触氧气条件下均能保持颜色稳定,且水溶性佳,并有较好的防腐效果。
本发明所述的防腐剂组合物由占组合物总重量5~35%的有机酸、0.05~2%的稳定剂、10~40%的增溶剂、1~20%的协同增效剂及20~80%的溶剂组成;各组分含量之和为100%。
所述防腐剂组合物中有机酸含量优选为10~30%。
所述防腐剂组合物中稳定剂含量优选为0.2~1%。
所述防腐剂组合物中增溶剂含量优选为20~30%。
所述防腐剂组合物中协同增效剂含量优选为5~15%。
所述防腐剂组合物中溶剂含量优选为40~65%。
所述防腐剂组合物中的有机酸为山梨酸或山梨酸与苯甲酸、脱氢乙酸、水杨酸中的至少一种的混合物。
所述防腐剂组合物中稳定剂为维生素C、维生素C磷酸酯钠、丁基羟基茴香醚、2,6-二叔丁基对甲酚、没食子酸丙酯、维生素E、维生素E醋酸酯、3,3’-硫代二丙酸二月桂酯中的一种与柠檬酸(盐)的混合物,且该混合物中柠檬酸(盐)与抗氧化剂的比例(重量比)为1∶(1~2)。该混合物比单独使用柠檬酸(盐)或一种抗氧化剂防山梨酸变色的效果更明显。
所述防腐剂组合物中增溶剂为聚氧乙烯(n1)蓖麻油、聚氧乙烯(n2)氢化蓖麻油、脂肪醇聚氧乙烯醚、烷基酚聚氧乙烯醚中的一种或两种的混合物。选用聚氧乙烯(n1)蓖麻油或聚氧乙烯(n2)氢化蓖麻油时,分子中聚氧乙烯的聚合度n1或n2一般为35~60;选用脂肪醇聚氧乙烯醚时一般为AEO9;选用烷基酚聚氧乙烯醚时一般为NP-10或OP-10。
所述防腐剂组合物中协同增效剂为1,2-戊二醇、1,2-己二醇、1,2-辛二醇、1,2-癸二醇、乙基己基甘油、辛酰羟肟酸、甘油辛酸酯、辛酰甘氨酸、聚赖氨酸中的一种或两种的混合物。
所述防腐剂组合物中溶剂为1,2-丙二醇、1,3-丙二醇、甲基丙二醇、二丙二醇、1,3-丁二醇、2,3-丁二醇、聚乙二醇200、聚乙二醇400、碳酸丙二醇酯、苯氧乙醇、苯甲醇中的一种或至少两种的混合物。
本发明提出的防腐剂组合物很容易制备,使用所属技术领域技术人员公知的方法,将有机酸、稳定剂、增溶剂、协同增效剂及溶剂在一定温度(30~60℃)下,按规定比例搅拌混合形成均相溶液即可。
本发明所述的防腐剂组合物在高温、光照和接触氧气条件下,均能保持颜色稳定。
本发明所述的防腐剂组合物在温度60℃(200小时)、90℃(80小时),均能保持颜色稳定。
本发明所述的防腐剂组合物在光照强度6000Lux、时间10天,均能保持颜色稳定。
本发明所述的防腐剂组合物在连续通入氧气情况下、时间1~8小时,均能保持颜色稳定。
本发明所述的防腐剂组合物在使用浓度下可完全水溶,在常温和低温下,不浑浊、无沉淀析出。
本发明所述的防腐剂组合物因组分间的协同效应,使山梨酸的颜色稳定性、水溶性大大提高,防腐能力也明显改善,可广泛应用于化妆品、家居洗涤用品、湿巾等产品领域。
具体实施方式
以下所述实施例详细说明了本发明,见表1。在这些实施例中,所有用量和比例均按重量计。
实施例1
表1.组合物各组分含量(%)
在带搅拌、温度计的200mL三口瓶中,按表1各组分含量计算的投料量,加入溶剂、协同增效剂、增溶剂、有机酸和稳定剂,搅拌下加热至50℃左右,使固体完全溶解,溶液澄清透明,降至室温,即得到颜色稳定的含山梨酸的防腐剂组合物。所得组合物在高温、光照和接触氧气条件下,均能保持颜色稳定,且水溶性佳,并有较好的防腐效果。
实施例2
将实施例1中组合物3#、6#和9#,不加稳定剂,用溶剂替代,得到相对应的对照组合物3-0#、6-0#和9-0#,将对照组合物、实施例1中的相应及其它部分组合物放入恒温恒湿箱中,进行在高温下颜色稳定性的考察。结果见表2、3。
表2.各组合物在高温(60℃)下的颜色稳定性
表2结果显示,在温度60℃、时间200小时条件下,含有稳定剂的组合物比不含稳定剂的组合物,颜色更稳定,具有更加优异的颜色稳定性。
表3.各组合物在高温(90℃)下的颜色稳定性
表3结果显示,在温度90℃、时间80小时条件下,含有稳定剂的组合物比不含稳定剂的组合物,颜色更稳定,具有更加优异的颜色稳定性。
实施例3
将实施例1中组合物3#、6#和9#,不加稳定剂,用溶剂替代,得到相对应的对照组合物3-0#、6-0#和9-0#,将对照组合物、实施例1中的相应及其它部分组合物放入光照培养箱中,进行在光照条件下颜色稳定性的考察。结果见表4。
表4.各组合物在光照(强度6000Lux)下的颜色稳定性
表4结果显示,在光照强度6000Lux、时间10天条件下,含有稳定剂的组合物比不含稳定剂组合物,颜色更稳定,具有更加优异的颜色稳定性。
实施例4
将实施例1中组合物3#、6#和7#,分别调整稳定剂比例、不加稳定剂用溶剂替代及只加入一种稳定剂,得到相对应的对照组合物,见表5。取对照组合物、实施例1中的相应及其它部分组合物各100mL,分别放入200mL三角瓶中,45~50℃水浴,以1L/min的进气量通入氧气,记录各组合物在相同时间内通氧气条件下的颜色变化,考察颜色稳定性。结果见表6。
表5.组合物各组分含量(%)
表6.各组合物在通氧气条件下的颜色稳定性
从表6的结果可以看出,在通入氧气情况下,不加稳定剂的组合物很易变色,颜色稳定性较差;单独的抗氧化剂或柠檬酸(盐)都具有一定的防组合物变色效果;但抗氧化剂与柠檬酸(盐)的二元稳定剂防变色效果更好,且柠檬酸(盐)与抗氧化剂的比例(重量比)为1∶(1~2)的稳定剂效果更出色,二者协同作用最佳。说明本发明组合物在接触氧气条件下具有优异的颜色稳定性。
实施例5
将山梨酸以10%、20%的浓度简单用溶剂溶解配成溶液,得到对照样品2-0#和4-0#,见表7。将对照样品、实施例1中的组合物,按照1.5%的添加量加入到水中,常温(20℃)搅拌下观察其在水中的溶解情况。结果见表8。
表7.对照样品组分含量(%)
表8.各组合物在水中的溶解情况
表8结果显示,本发明组合物可以大大提高山梨酸等有机酸在水中的实际溶解度,仅通过简单溶剂溶解并不能明显改善山梨酸在水中的溶解性能。本发明组合物在正常添加量下完全可以满足山梨酸的实际应用需要。
实施例6
通过平板涂布法(对霉菌、酵母菌)及稀释培养法(对细菌),将山梨酸纯品、实施例5中的对照样品及实施例1中的部分相关组合物进行微生物最小抑菌浓度(MIC值)测试,结果见表9。
表9.各组合物MIC值
表9结果显示,与对照样品比较,在等效的山梨酸活性物浓度下,本发明组合物的实际抑菌能力要优于单独的山梨酸纯品或简单溶剂溶解的对照样品。说明本发明组合物组分间具有较好的协同增效作用,防腐效果更佳。
实施例7
本发明所述的防腐剂组合物可用于各种化妆品,包括洗去型产品(如洗面奶、洗发水、沐浴露、洗手液、牙膏等)和驻留型产品(如膏霜、乳液、爽肤水、面膜等);也可用于家居洗涤用品(如餐具洗涤剂、洗衣液、厨卫清洁剂等);还可用于各类湿巾中。表10为实施例1中的组合物应用于各种类型产品的添加量情况。
表10.本发明组合物应用于各种产品的添加量情况
Claims (14)
1.一种颜色稳定的含山梨酸的防腐剂组合物,其特征在于:由占组合物总重量5~35%的有机酸、0.05~2%的稳定剂、10~40%的增溶剂、1~20%的协同增效剂及20~80%的溶剂组成。
2.根据权利要求1所述的防腐剂组合物,其特征在于:所述有机酸为山梨酸或山梨酸与苯甲酸、脱氢乙酸、水杨酸中的至少一种的混合物。
3.根据权利要求1所述的防腐剂组合物,其特征在于:所述稳定剂为维生素C、维生素C磷酸酯钠、丁基羟基茴香醚、2,6-二叔丁基对甲酚、没食子酸丙酯、维生素E、维生素E醋酸酯、3,3’-硫代二丙酸二月桂酯中的一种与柠檬酸(盐)的混合物。
4.根据权利要求3所述的防腐剂组合物,其特征在于:所述稳定剂混合物中柠檬酸(盐)与其它一种稳定剂的比例(重量比)为1∶(1~2)。
5.根据权利要求1所述的防腐剂组合物,其特征在于:所述增溶剂为聚氧乙烯(n1)蓖麻油、聚氧乙烯(n2)氢化蓖麻油、脂肪醇聚氧乙烯醚、烷基酚聚氧乙烯醚中的一种或两种的混合物。
6.根据权利要求5所述的防腐剂组合物,其特征在于:所述聚氧乙烯(n1)蓖麻油或聚氧乙烯(n2)氢化蓖麻油中的聚氧乙烯的聚合度n1或n2为35~60;脂肪醇聚氧乙烯醚为AEO9;烷基酚聚氧乙烯醚为NP-10或OP-10。
7.根据权利要求1所述的防腐剂组合物,其特征在于:所述协同增效剂为1,2-戊二醇、1,2-己二醇、1,2-辛二醇、1,2-癸二醇、乙基己基甘油、辛酰羟肟酸、甘油辛酸酯、辛酰甘氨酸、聚赖氨酸中的一种或两种的混合物。
8.根据权利要求1所述的防腐剂组合物,其特征在于,所述溶剂为1,2-丙二醇、1,3-丙二醇、甲基丙二醇、二丙二醇、1,3-丁二醇、2,3-丁二醇、聚乙二醇200、聚乙二醇400、碳酸丙二醇酯、苯氧乙醇、苯甲醇中的一种或至少两种的混合物。
9.根据权利要求1或2所述的防腐剂组合物,其特征在于:所述有机酸占组合物总重量的10~30%。
10.根据权利要求1或3或4所述的防腐剂组合物,其特征在于:所述稳定剂占组合物总重量的0.2~1%。
11.根据权利要求1或5或6所述的防腐剂组合物,其特征在于:所述增溶剂占组合物总重量的20~30%。
12.根据权利要求1或7所述的防腐剂组合物,其特征在于:所述协同增效剂占组合物总重量的5~15%。
13.根据权利要求1或8所述的防腐剂组合物,其特征在于:所述溶剂占组合物总重量的40~65%。
14.根据权利要求1~13任一所述的防腐剂组合物在化妆品、家居洗涤用品、湿巾中的用途。
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