月桂酸类代可可脂巧克力起霜机理及品质改善
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摘要
月桂酸类代可可脂（CBS）具有与可可脂相似的物理性质，并且来源广泛、价格低廉，可取代可可脂用于巧克力的生产，在糖果巧克力产品中具有广阔的应用前景，但因CBS巧克力容易出现起霜现象而导致其原有的光滑亮泽、入口即溶的特性被破坏，成为影响糖果巧克力工业的一大难题。本课题围绕CBS巧克力的起霜问题开展研究，结合静态和动态分析推测起霜机制，并对基料油脂、分散相与巧克力物性之间的构效关系进行探讨，用以指导添加乳化剂改善基料油脂结晶特性并延缓霜的形成。主要研究内容和取得的
研究成果如下：
1、采用原子力显微镜（AFM）、扫描电镜（SEM）和超景深三维显微镜为表征手段，对新鲜和起霜的CBS巧克力的表面形貌和微观组织结构进行分析，之后在不破坏其晶体结构的控温条件下对霜与基质进行分离，分析其甘油三酯（TAG）组成、熔化性质、同质多晶和晶体形态，并用X-射线衍射（XRD）动态分析了温度波动过程中模型巧克力样品的同质多晶型转变，结果表明：新鲜巧克力表面油脂晶体均匀分布，形成结晶网络，将其它组分锁定在网络结构内部；起霜巧克力表面粗糙，油相与分散相发生分离，部分油脂晶体聚集并伸出巧克力表面散射光线，使巧克力表面呈现起霜状态；与基质相比，霜中三饱和TAG含量降低19.7%，单不饱和TAG的含量增加130.1%，霜的晶型为β晶型与β′晶型共存，而巧克力基质中仍呈β′晶型，温度波动6周试验结果表明巧克力中未发生晶型转变。
2、选用氢化棕榈仁软脂（HPKO）和氢化棕榈仁硬脂（HPKS）这两种常用的CBS以及可可脂（CB）和乳脂（MF）作为基料油，对其混合体系的相行为进行了系统分析，并探讨了基料油脂相行为与巧克力品质的构效关系，结果表明：CBS与CB相容性差，共晶作用明显，HPKO与CB的相容性优于HPKS与CB的相容性；CBS/MF二元体系呈现固溶体状态，MF的稀释作用使体系SFC值降低；CBS/CB/MF三元混合体系中，CB和MF添加量均不大于10%时，经调温处理的混合体系呈现β′晶型。基料油脂的SFC值影响模型巧克力的硬度，对于HPKS体系而言，SFC值与硬度呈线性相关。模型巧克力的起霜现象与基料油的相容性密切相关，CBS/CB/MF三元体系中，稀释作用对HPKO/CB/MF体系影响更大，添加10%CB的巧克力在储存11周以上时出现薄雾状霜，共晶作用对HPKS/CB/MF体系的影响高于稀释作用，5%CB添加量的样品在储存4周之后巧克力表面迅速出现白斑状霜。
3、采用SEM和DSC为表征手段，考察了可可粉、糖（结晶糖和糖粉）、奶粉（全脂奶粉和脱脂奶粉）三种分散相对基料油脂熔化结晶性质的影响，并对结晶曲线进行了动力学的分析，结果表明：分散相对体系的熔化性质具有显著影响，可可粉能为基料油的结晶提供非均匀成核位点，从而促进体系稳定晶型的形成，使体系的结晶峰温度升高约3℃；与结晶糖相比，糖粉混合体系结晶焓值高出20J/g；脱脂奶粉可促进基料油脂形成陡峭的熔化结晶峰，而全脂奶粉不仅使体系的熔程变宽，而且使熔化和结晶焓值降低。卵磷脂的添加降低了可可粉和糖粉与基料油脂混合体系的结晶温度，而使脱脂奶粉混合体系中基料油脂的结晶温度升高约0.4℃。Avrami指数n值的结果表明，糖的添加使n值由3.4增加至4.4~7.4，晶体向多维空间生长；可可粉使基料油体系的n值降低，但随着卵磷脂的加入这种作用消失；全脂奶粉未改变晶体生长机制，脱脂奶粉使体系变为零星成核的球状生长。
4、在上述研究分析的基础上，推测CBS巧克力的起霜机理为：CBS巧克力体系中固体脂肪与液态油脂共存，储存过程中，在体系过冷度的作用下，部分液态油脂附着晶体表面使晶体不断生长，可可脂的TAG晶体晶格较大，CBS的TAG晶体晶格较小，两者相互排斥并逐渐分离，同类型TAG分子之间结晶网络进一步密化，而液态油脂在体系内自由迁移；随储存时间的延长，不同类型的TAG分子进一步分离，使分散相颗粒之间在范德华作用力的推动下逐渐靠近，并最终聚集，油相与分散相分离，油相中可可脂和CBS的TAG晶体分离，可可脂中的对称型单不饱和TAG及CBS中的三月桂酸TAG随液态油脂逐渐向表面迁移，并发生同质多晶型转变，伸出巧克力表面而形成霜。
5、选用卵磷脂、单甘酯、PGPR、span60、tween60五种常用乳化剂考察其对基料油脂结晶性质的影响，在此基础上筛选卵磷脂、单甘酯和span60三种乳化剂制备模型巧克力，考察其单一添加量分别为0.5%、1.0%和1.5%，及1.0%总添加量下按1:3、1:1和3:1两两复配时对巧克力物性的影响，并用结晶热力学、结晶动力学方法对此进行了理论分析，结果表明：乳化剂的添加导致基料油脂的成核和晶体生长机制发生改变，其中span60及单甘酯使基料油瞬时成核，并促进晶体以二维平面上的盘状形式生长；乳化剂种类和添加量均对巧克力物性产生显著影响，卵磷脂的添加可显著改善体系的流变性质；单甘酯添加量增加，体系软化作用增强；span60的添加可以使巧克力在16周的储存期内白化指数不发生明显变化，但流变性质表明其屈服值、表观黏度和触变性值均较高，不利于巧克力的加工操作，与单甘酯或卵磷脂分别以3:1比例复配时既有较好的流变性质，同时具有较好的延缓起霜作用。
Since its physical properties resembling those of cocoa butter (CB), as well as its widely cheap sources, lauriccocoa butter substitute (CBS) becomes an important material which has an extensive application prospect in theconfectionery industry. CBS, which doesn’t need tempering when processing, can be used in place of a major part ofCB that is present in normal chocolate and endue the chocolate with good glossiness. However, bloom formation, aworldwide difficulty in confectionery industry, is one of the outstanding problems of these chocolate products. Thisresearch focused on the bloom problem of CBS chocolate, speculated the mechanism by using static and dynamicanalysis, then discussed the correlation among based fat, dispersed phase and the physical properties of chocolate,finally evaluated the contribution of emulsifiers on modifying the crystallization properties of based fat, as well as theireffects on delaying the bloom formation. The main results are as follows:
1. The morphological and microstructure properties of fresh and bloom chocolate were evaluated by using atomicforce microscopy (AFM), scanning electric microscopy (SEM), and extended depth-of-field3-dimension microscopymethods. Bloom and chocolate matrix were carefully separated without destroying the crystallization to determine theirtriacylglycerol (TAG) composition, melting curve, polymorphism transformation, and crystallize shape. The resultsshowed that: fat crystals evenly distributed on the fresh chocolate surface, forming a dense crystal network, othercomponents were locked inside the network. Bloomed chocolate showed a coarse surface, phase separation occurredbetween fat phase and the dispersed phase, some fat crystals aggregated and outreached from the chocolate surface,scattered light leading to bloom appearance. Compared with the chocolate matrix, bloom showed a decline of saturatedTAG and increment of monounsaturated TAG,19.7%and130.1%separately. Polymorphism results showed acombination of β and β′forms for bloom while a β′form for chocolate matrix. XRD results of model chocolate after6weeks temperature fluctuation storage showed that no polymorphism translation appeared among the chocolate.
2. Phase behaviors of CBS (two typical types, hydrogenated palm kernel olein (HPKO) and hydrogenated palmkernel stearin (HPKS)), cocoa butter (CB), and milk fat (MF) were systematic analyzed, meanwhile its correlation withmodel chocolate properties were evaluated. Both CBS/CB binary blends displayed significant eutectic behaviors, butHPKO showed better incorporation with CB than HPKS. Dilution effect was observed in both CBS/MF blends,indicated that MF decreased the solid fat content (SFC) of CBS. For the ternary mixtures of CBS/CB/MF, when CB andMF addition were both under10%, the mixture showed a β′form. SFC showed a relationship with the chocolatehardness, for the HPKS based model chocolate, there was a linear correlation between SFC and hardness. Bloomformation closely related with the phase behavior of based fat, for the HPKO/CB/MF ternary mixtures, in which thedilution effect significantly affected the system, a mist-like bloom was induced after11weeks storage, while eutecticshowed a more significant impact on the HPKS/CB/MF mixture than dilution effect, with5%CB addition, a largewhite spot-like bloom was induced after4weeks storage.
3. SEM and DSC were introduced to determine the effect of dispersed phase particles on the fat crystallization,meanwhile, dynamic analysis were done for the crystallize curve. The dispersed particles had a significant effect on themelting properties of the system. Cocoa powder could provide heterogeneous nucleation sites for the fat crystals andinduce a stable polymorphism formation, leading to the crystallize temperature increased3oC; crystallization enthalpyof sugar powder was20J/g higher than that of crystal sugar; skim milk powder promoted steep melting andcrystallizing peaks, while whole milk powder showed a broad melting range with low melting enthalpy. Addition oflecithin decreased the crystallizing temperature of both cocoa powder fat mixture and sugar fat mixture, but increasedthe crystallizing temperature (0.4oC) of milk powder fat mixture. The Avrami n value indicated that, sugar increased nfrom3.4to4.4~7.4, inducing a multidimensional space growth; cocoa powder decreased the n value, although thisdecrease effect disappeared with the addition of lecithin; whole milk powder did not change the nuclear and crystalgrowth mechanism, while skim milk powder changed the crystallization to spherical growth with a sporadic nucleation.
4. These results suggested that the mechanism of bloom formation in CBS chocolate was as follows: both fatcrystals and liquid oil existed in the CBS chocolate system, during storage, fat crystals kept growth under the drivingforce of the subcooling, crystal lattice of CB was larger than that of CBS, they tended to separate from each other, thesame crystals gathered to form new dense network, while liquid oil migrated freely inside the system; along with thefurther separation of CB and CBS crystals, dispersed particles became more close and finally aggregated under thedriving of van der waals forces, fat phase and dispersed phase separated from each other, among the fat phase TAG ofCB and CBS separated from each other, migration liquid oil brought the CB TAG and CBS LLL (trilaurin) to thesurface of chocolate, with a polymorphism transformation, then large crystals outreached from the surface.
5. Five types of emulsifiers were chosen to evaluate their effects on the based fat crystallization, three additionlevels,0.5%,1.0%, and1.5%, for single emulsifier and three ratios,1:3,1:1, and3:1, for combination of emulsifierwere chosen to evaluate their effects on model chocolates by crystallization thermal dynamics and crystallizationkinetics analysis. Addition of emulsifiers changed the nucleation and crystal growth mechanisms of based fat, amongwhich span60and monoglyceride accelerated the nucleation speed, and promoted the two dimension plate growth ofcrystallization. Emulsifier type and additional level also affected the physical properties of chocolate. Addition oflecithin significantly improved the rheology property of molten chocolate; monoglyceride softened the model chocolate,as the additional level increased, the soften effect increased; addition of span60showed a bloom delay effect within16weeks storage, however, its yield stress, apparent viscosity, and thixotropism were high, which had a negative impact on the processing procedure, when molten chocolate was combined with monoglyceride or lecithin in ratios of3:1, itsrheological properties were improved, and also had an effectively bloom delay effect.
研究成果如下：
1、采用原子力显微镜（AFM）、扫描电镜（SEM）和超景深三维显微镜为表征手段，对新鲜和起霜的CBS巧克力的表面形貌和微观组织结构进行分析，之后在不破坏其晶体结构的控温条件下对霜与基质进行分离，分析其甘油三酯（TAG）组成、熔化性质、同质多晶和晶体形态，并用X-射线衍射（XRD）动态分析了温度波动过程中模型巧克力样品的同质多晶型转变，结果表明：新鲜巧克力表面油脂晶体均匀分布，形成结晶网络，将其它组分锁定在网络结构内部；起霜巧克力表面粗糙，油相与分散相发生分离，部分油脂晶体聚集并伸出巧克力表面散射光线，使巧克力表面呈现起霜状态；与基质相比，霜中三饱和TAG含量降低19.7%，单不饱和TAG的含量增加130.1%，霜的晶型为β晶型与β′晶型共存，而巧克力基质中仍呈β′晶型，温度波动6周试验结果表明巧克力中未发生晶型转变。
2、选用氢化棕榈仁软脂（HPKO）和氢化棕榈仁硬脂（HPKS）这两种常用的CBS以及可可脂（CB）和乳脂（MF）作为基料油，对其混合体系的相行为进行了系统分析，并探讨了基料油脂相行为与巧克力品质的构效关系，结果表明：CBS与CB相容性差，共晶作用明显，HPKO与CB的相容性优于HPKS与CB的相容性；CBS/MF二元体系呈现固溶体状态，MF的稀释作用使体系SFC值降低；CBS/CB/MF三元混合体系中，CB和MF添加量均不大于10%时，经调温处理的混合体系呈现β′晶型。基料油脂的SFC值影响模型巧克力的硬度，对于HPKS体系而言，SFC值与硬度呈线性相关。模型巧克力的起霜现象与基料油的相容性密切相关，CBS/CB/MF三元体系中，稀释作用对HPKO/CB/MF体系影响更大，添加10%CB的巧克力在储存11周以上时出现薄雾状霜，共晶作用对HPKS/CB/MF体系的影响高于稀释作用，5%CB添加量的样品在储存4周之后巧克力表面迅速出现白斑状霜。
3、采用SEM和DSC为表征手段，考察了可可粉、糖（结晶糖和糖粉）、奶粉（全脂奶粉和脱脂奶粉）三种分散相对基料油脂熔化结晶性质的影响，并对结晶曲线进行了动力学的分析，结果表明：分散相对体系的熔化性质具有显著影响，可可粉能为基料油的结晶提供非均匀成核位点，从而促进体系稳定晶型的形成，使体系的结晶峰温度升高约3℃；与结晶糖相比，糖粉混合体系结晶焓值高出20J/g；脱脂奶粉可促进基料油脂形成陡峭的熔化结晶峰，而全脂奶粉不仅使体系的熔程变宽，而且使熔化和结晶焓值降低。卵磷脂的添加降低了可可粉和糖粉与基料油脂混合体系的结晶温度，而使脱脂奶粉混合体系中基料油脂的结晶温度升高约0.4℃。Avrami指数n值的结果表明，糖的添加使n值由3.4增加至4.4~7.4，晶体向多维空间生长；可可粉使基料油体系的n值降低，但随着卵磷脂的加入这种作用消失；全脂奶粉未改变晶体生长机制，脱脂奶粉使体系变为零星成核的球状生长。
4、在上述研究分析的基础上，推测CBS巧克力的起霜机理为：CBS巧克力体系中固体脂肪与液态油脂共存，储存过程中，在体系过冷度的作用下，部分液态油脂附着晶体表面使晶体不断生长，可可脂的TAG晶体晶格较大，CBS的TAG晶体晶格较小，两者相互排斥并逐渐分离，同类型TAG分子之间结晶网络进一步密化，而液态油脂在体系内自由迁移；随储存时间的延长，不同类型的TAG分子进一步分离，使分散相颗粒之间在范德华作用力的推动下逐渐靠近，并最终聚集，油相与分散相分离，油相中可可脂和CBS的TAG晶体分离，可可脂中的对称型单不饱和TAG及CBS中的三月桂酸TAG随液态油脂逐渐向表面迁移，并发生同质多晶型转变，伸出巧克力表面而形成霜。
5、选用卵磷脂、单甘酯、PGPR、span60、tween60五种常用乳化剂考察其对基料油脂结晶性质的影响，在此基础上筛选卵磷脂、单甘酯和span60三种乳化剂制备模型巧克力，考察其单一添加量分别为0.5%、1.0%和1.5%，及1.0%总添加量下按1:3、1:1和3:1两两复配时对巧克力物性的影响，并用结晶热力学、结晶动力学方法对此进行了理论分析，结果表明：乳化剂的添加导致基料油脂的成核和晶体生长机制发生改变，其中span60及单甘酯使基料油瞬时成核，并促进晶体以二维平面上的盘状形式生长；乳化剂种类和添加量均对巧克力物性产生显著影响，卵磷脂的添加可显著改善体系的流变性质；单甘酯添加量增加，体系软化作用增强；span60的添加可以使巧克力在16周的储存期内白化指数不发生明显变化，但流变性质表明其屈服值、表观黏度和触变性值均较高，不利于巧克力的加工操作，与单甘酯或卵磷脂分别以3:1比例复配时既有较好的流变性质，同时具有较好的延缓起霜作用。
Since its physical properties resembling those of cocoa butter (CB), as well as its widely cheap sources, lauriccocoa butter substitute (CBS) becomes an important material which has an extensive application prospect in theconfectionery industry. CBS, which doesn’t need tempering when processing, can be used in place of a major part ofCB that is present in normal chocolate and endue the chocolate with good glossiness. However, bloom formation, aworldwide difficulty in confectionery industry, is one of the outstanding problems of these chocolate products. Thisresearch focused on the bloom problem of CBS chocolate, speculated the mechanism by using static and dynamicanalysis, then discussed the correlation among based fat, dispersed phase and the physical properties of chocolate,finally evaluated the contribution of emulsifiers on modifying the crystallization properties of based fat, as well as theireffects on delaying the bloom formation. The main results are as follows:
1. The morphological and microstructure properties of fresh and bloom chocolate were evaluated by using atomicforce microscopy (AFM), scanning electric microscopy (SEM), and extended depth-of-field3-dimension microscopymethods. Bloom and chocolate matrix were carefully separated without destroying the crystallization to determine theirtriacylglycerol (TAG) composition, melting curve, polymorphism transformation, and crystallize shape. The resultsshowed that: fat crystals evenly distributed on the fresh chocolate surface, forming a dense crystal network, othercomponents were locked inside the network. Bloomed chocolate showed a coarse surface, phase separation occurredbetween fat phase and the dispersed phase, some fat crystals aggregated and outreached from the chocolate surface,scattered light leading to bloom appearance. Compared with the chocolate matrix, bloom showed a decline of saturatedTAG and increment of monounsaturated TAG,19.7%and130.1%separately. Polymorphism results showed acombination of β and β′forms for bloom while a β′form for chocolate matrix. XRD results of model chocolate after6weeks temperature fluctuation storage showed that no polymorphism translation appeared among the chocolate.
2. Phase behaviors of CBS (two typical types, hydrogenated palm kernel olein (HPKO) and hydrogenated palmkernel stearin (HPKS)), cocoa butter (CB), and milk fat (MF) were systematic analyzed, meanwhile its correlation withmodel chocolate properties were evaluated. Both CBS/CB binary blends displayed significant eutectic behaviors, butHPKO showed better incorporation with CB than HPKS. Dilution effect was observed in both CBS/MF blends,indicated that MF decreased the solid fat content (SFC) of CBS. For the ternary mixtures of CBS/CB/MF, when CB andMF addition were both under10%, the mixture showed a β′form. SFC showed a relationship with the chocolatehardness, for the HPKS based model chocolate, there was a linear correlation between SFC and hardness. Bloomformation closely related with the phase behavior of based fat, for the HPKO/CB/MF ternary mixtures, in which thedilution effect significantly affected the system, a mist-like bloom was induced after11weeks storage, while eutecticshowed a more significant impact on the HPKS/CB/MF mixture than dilution effect, with5%CB addition, a largewhite spot-like bloom was induced after4weeks storage.
3. SEM and DSC were introduced to determine the effect of dispersed phase particles on the fat crystallization,meanwhile, dynamic analysis were done for the crystallize curve. The dispersed particles had a significant effect on themelting properties of the system. Cocoa powder could provide heterogeneous nucleation sites for the fat crystals andinduce a stable polymorphism formation, leading to the crystallize temperature increased3oC; crystallization enthalpyof sugar powder was20J/g higher than that of crystal sugar; skim milk powder promoted steep melting andcrystallizing peaks, while whole milk powder showed a broad melting range with low melting enthalpy. Addition oflecithin decreased the crystallizing temperature of both cocoa powder fat mixture and sugar fat mixture, but increasedthe crystallizing temperature (0.4oC) of milk powder fat mixture. The Avrami n value indicated that, sugar increased nfrom3.4to4.4~7.4, inducing a multidimensional space growth; cocoa powder decreased the n value, although thisdecrease effect disappeared with the addition of lecithin; whole milk powder did not change the nuclear and crystalgrowth mechanism, while skim milk powder changed the crystallization to spherical growth with a sporadic nucleation.
4. These results suggested that the mechanism of bloom formation in CBS chocolate was as follows: both fatcrystals and liquid oil existed in the CBS chocolate system, during storage, fat crystals kept growth under the drivingforce of the subcooling, crystal lattice of CB was larger than that of CBS, they tended to separate from each other, thesame crystals gathered to form new dense network, while liquid oil migrated freely inside the system; along with thefurther separation of CB and CBS crystals, dispersed particles became more close and finally aggregated under thedriving of van der waals forces, fat phase and dispersed phase separated from each other, among the fat phase TAG ofCB and CBS separated from each other, migration liquid oil brought the CB TAG and CBS LLL (trilaurin) to thesurface of chocolate, with a polymorphism transformation, then large crystals outreached from the surface.
5. Five types of emulsifiers were chosen to evaluate their effects on the based fat crystallization, three additionlevels,0.5%,1.0%, and1.5%, for single emulsifier and three ratios,1:3,1:1, and3:1, for combination of emulsifierwere chosen to evaluate their effects on model chocolates by crystallization thermal dynamics and crystallizationkinetics analysis. Addition of emulsifiers changed the nucleation and crystal growth mechanisms of based fat, amongwhich span60and monoglyceride accelerated the nucleation speed, and promoted the two dimension plate growth ofcrystallization. Emulsifier type and additional level also affected the physical properties of chocolate. Addition oflecithin significantly improved the rheology property of molten chocolate; monoglyceride softened the model chocolate,as the additional level increased, the soften effect increased; addition of span60showed a bloom delay effect within16weeks storage, however, its yield stress, apparent viscosity, and thixotropism were high, which had a negative impact on the processing procedure, when molten chocolate was combined with monoglyceride or lecithin in ratios of3:1, itsrheological properties were improved, and also had an effectively bloom delay effect.
引文
1.蔡云升,张文治.新版糖果巧克力配方[M].北京:中国轻工业出版社,2002.
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