CN111738548A - 一种茉莉花茶香气品质评价方法及其应用 - Google Patents
一种茉莉花茶香气品质评价方法及其应用 Download PDFInfo
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Abstract
本发明一种茉莉花茶香气品质评价方法，属于茶叶技术领域。所述的评价方法是根据(顺式‑3‑己烯醇苯甲酸酯+吲哚+氨茴酸甲酯)含量/(芳樟醇+乙酸叶醇酯+乙酸卞酯)含量，这一比值的大小判断茉莉花茶的品质。本发明建立的茉莉花茶品质评价的新指数对花茶香气品质评价的准确度和区分度好，且客观、准确、不受人为因素影响，有利于促进花茶产业标准化发展。
Description
技术领域
本发明属于茶叶品质评价技术领域，具体涉及一种茉莉花茶香气品质评价方法，及其在不同地区、不同形状茉莉花茶品质评价中的应用。
背景技术
茉莉花茶是将茶坯和茉莉鲜花拼合，由茶坯吸附鲜花香气窨制而成。花茶品质评价以感官审评为主，但感官审评受审评人员技能、评审环境等因素的影响，不可避免地产生误差，存在审评不够客观、科学的问题，而且感官审评过程繁琐复杂、耗时长，成本高。因此，建立科学有效的花茶品质评价方法，对于保证产品质量稳定性、促进产业标准化生产具有重要意义。
茶叶的感官特征(色、香、味)是其内含物质的外在表现，利用茶叶内含物质化学指纹图谱模型可将感官指标量化。花茶品质取决于香气，在感官评审中香气权重为40％。目前，已有许多应用香气质量指纹图谱模型方法评价花茶品质的报道，采用判别模型的方法建立茉莉花茶香气质量模型，进行花茶等级评判，与感官审评结果具有很好的一致性，但是应用模型判断较为麻烦，无法实现快速评价。
研究表明，茉莉花茶香气成分主要由酯类、醇类和萜烯类化合物组成，国内外已展开了花茶香气成分与品质的相关性研究，如Yamanishi等(Yamanishi,T.Aroma of ChineseScented Green Tea.In Frontiers of FlaVor.Proceedings of 5th InternationalFlavor Conference,Porto Karras,Chalkidiki,Greece,July 1–3,1987[C].Amsterdam,1987.)认为茉莉花茶的品质与芳樟醇/(苯甲醇+乙酸苄酯+苯甲酸-3-己烯酯+苯甲酸甲酯+氨茴酸甲酯)的浓度比值呈负相关；陆宁等(陆宁等.茉莉花茶香气成分与品质之间关系的初步研究[J].食品科学,2004,25(6):93-97.)认为芳樟醇、乙酸苄酯、顺-3-己烯醇和水杨酸甲酯与花茶香气品质呈正相关；Lin等(Lin J,et al.A Novel Quality EvaluationIndex and Strategies to Identify Scenting Quality of Jasmine Tea Based onHeadspace Volatiles Analysis[J].Food Sci Biotec,2013,22:331～340)认为茉莉花茶香气品质可利用JTF指数{JTF＝(α-法呢烯+苯甲酸-3-己烯酯+氨茴酸甲酯+吲哚)含量/芳樟醇含量}来评价，JTF数值越大，花茶的等级越高。但是，这些方法仅能区分花茶品质高低明显的样本，对级别判定不准确。
因此，有必要建立茉莉花茶香气品质评价新指标，对不同品质花茶进行准确分级，为花茶品质评价提供客观有效的方法。
发明内容
为了解决茉莉花茶准确分级的问题，发明人建立了一种茉莉花茶香气品质评价新指标。技术方案如下：
一种茉莉花茶香气品质评价方法，根据(顺式-3-己烯醇苯甲酸酯+吲哚+氨茴酸甲酯)含量/(芳樟醇+乙酸叶醇酯+乙酸卞酯)含量，这一比值的大小判断茉莉花茶的品质。
所述的评价方法包括如下步骤：
采用顶空固相微萃取方法富集花茶香气成分；
利用GC-MS技术测定茉莉花茶香气组成；
构建茉莉花茶香气品质的计算公式，即XFJTF得分＝(顺式-3-己烯醇苯甲酸酯+吲哚+氨茴酸甲酯)含量/(芳樟醇+乙酸叶醇酯+乙酸卞酯)含量×100；
根据茉莉花茶香气得分判断茉莉花茶的品质，将不同级别的茉莉花茶品质分为：低等，得分0-15分；中等，得分16-30分；高等，得分31-45分；优等，得分46-60分；特优等，得分≥61分。
其中，顶空固相微萃取方法包括如下步骤：
萃取头老化：萃取头用丙酮浸泡20-40min后，65μm聚二甲基硅氧烷/二乙烯基苯萃取头在240-260℃老化20-40min；
萃取条件：称取1-2g茶叶置于密封的顶空瓶中，60-70℃水浴5-10min后插入SPME纤维头吸附15-25min，240-260℃解吸3-5min。
GC-MS技术测定茉莉花茶香气组成的方法如下：
色谱条件：进样口温度240-260℃，柱温40-60℃；程序为：起始温度40-60℃，保持2-3min，以4-5℃/min升到120-130℃，保持15-20min，以4-5℃/min升到170-180℃，保持2-3min，以30-40℃/min升到280-290℃，保持2-3min；
质谱条件：离子源EI；采集模式为全扫描；溶剂延迟5-8min；EMV模式为相对值；质量扫描范围：25.00～550.00amu；MS离子源温度为220-240℃，MS四级杆温度140-160℃；
检测的化合物经谱库检索，同时采用线性升温公式计算各组分的实验保留指数，结合文献进行花茶香气成分鉴定；香气组分相对含量采用峰面积归一化法进行计算，表示为各香气组分的峰面积占总峰面积之比值。
进一步的，所述的香气成分包括醇类、酯类、含氮化合物和萜烯类化合物；其中，醇类化合物以芳樟醇和苯甲醇为主，酯类化合物以乙酸卞酯、乙酸叶醇酯、顺式-3-己烯醇苯甲酸酯和水杨酸甲酯为主，含氮化合物以吲哚和氨茴酸甲酯为主，萜烯类化合物以α-法呢烯为主。
进一步的，所述的茉莉花茶香气品质评价方法在福州茉莉花茶品质评价中的应用。
进一步的，所述的茉莉花茶香气品质评价方法在茉莉扁形茶或茉莉圆珠茶或茉莉条形茶品质评价中的应用。
区别于现有技术，上述技术方案的优点在于：
(1)本发明可以对不同品质花茶进行准确分级，为花茶品质评价提供客观有效的方法。
(2)本发明建立的XFJTF指数评价花茶品质的准确度和区分度更好。
(3)本发明建立的方法客观、准确、不受人为因素影响，有利于促进花茶产业标准化发展。
附图说明
图1为具体实施方式所述的不同级别福州茉莉花茶主成分分析。
具体实施方式
为详细说明技术方案的技术内容、构造特征、所实现目的及效果，以下结合具体实施例并配合附图详予说明。
实施例1
1.材料与方法
1.1试验材料
不同级别的福州茉莉花茶由福建东来茶业有限公司生产，茶样经质检后，根据品质进行定价。检验茶来源于当地市场和网络市场；茶王赛样本由福州市经济作物技术站提供。
1.2主要仪器
气相色谱-质谱联用仪7890A/5975C(美国安捷伦科技公司)；液相色谱1100(美国安捷伦科技公司)；萃取装置：SPME手动进样手柄、萃取头(65μm PDMS/DVB)。
1.3香气萃取
利用顶空固相微萃取方法富集花茶香气成分。萃取头老化：萃取头用丙酮浸泡30min后，65μm聚二甲基硅氧烷/二乙烯基苯(PDMS/DVB)萃取头在250℃老化30min。萃取条件：称取1g茶叶置于密封的顶空瓶中，65℃水浴5min后插入SPME纤维头吸附20分钟。于250℃解吸3min后进行GC-MS测定。
1.4香气测定
利用GC-MS技术测定茉莉花茶香气组成。色谱条件：进样口温度250℃，柱温50℃。程序为：起始温度50℃，保持2min，以5℃/min升到120℃，保持15min，以5℃/min升到180℃，保持2min，以30℃/min升到280℃，保持2min。质谱条件：离子源EI；采集模式为全扫描；溶剂延迟6min；EMV模式为相对值；质量扫描范围：25.00～550.00amu；MS离子源温度为230℃，MS四级杆温度150℃。正己烷稀释正构烷烃混合对照品，按上述色谱条件进行分析。
1.5定性与定量分析
检测的化合物经NIST谱库检索，同时采用线性升温公式计算各组分的实验保留指数(KI)，结合文献进行花茶香气成分鉴定。香气组分相对含量采用峰面积归一化法进行计算，表示为各香气组分的峰面积占总峰面积之比值。利用MPP和SPSS软件对香气数据进行主成分和聚类分析。
2.结果与分析
2.1不同级别的茉莉花茶香气成分组成
11个不同级别的福州茉莉花茶香气成分如表1所示。结果表明，从11个福州茉莉花茶中共鉴定出40个香气物质，包括5个醇类、11个酯类、3个含N化合物、17个萜烯类化合物和4个其他类化合物。醇类化合物以芳樟醇和苯甲醇为主；酯类化合物以乙酸卞酯、乙酸叶醇酯、顺式-3-己烯醇苯甲酸酯和水杨酸甲酯为主；含N化合物以吲哚和氨茴酸甲酯为主；萜烯类化合物以α-法呢烯为主。
表1 11个不同级别的茉莉花茶香气成分及其相对含量
注：“-”表示该物质未检测到。
根据Lin等提出的公式JTF＝(α-法呢烯+顺式-3-己烯醇苯甲酸酯+吲哚+氨茴酸甲酯)含量/芳樟醇含量，计算11个不同级别福州茉莉花茶的JTF指数，结果如表2所示。从表中可以看出，Y1、Y2、Y3和Y6茶样的JTF指数低于1，其中Y1茶样的JTF指数最低，Y9茶样JTF指数最高。将11个茶叶定价与JTF指数对照后，发现该指数只能区分低价和高价的花茶，区分率较差。
表2 11个不同级别的福州茉莉花茶香气评价指数JTF值
| 样本 | Y1 | Y2 | Y3 | Y4 | Y5 | Y6 | Y7 | Y8 | Y9 | Y10 | Y11 |
| 定价(元/斤) | 68 | 90 | 160 | 260 | 280 | 380 | 280 | 580 | 1080 | 1620 | 3800 |
| JTF值 | 0.49 | 0.70 | 0.82 | 1.01 | 1.07 | 0.93 | 1.16 | 1.37 | 1.82 | 1.34 | 1.58 |
2.2不同级别茉莉花茶香气成分主成分
在茉莉花茶实际生产过程中，有时为了提高茉莉花茶香味的浓度会加入玉兰“调香”，但优质茉莉花茶不应呈现玉兰味。研究表明，玉兰花的香气主要由醇类和萜烯类化合物组成，其中醇类化合物以甲醇和乙醇为主，萜烯类化合物中α-法呢烯的含量最高。茉莉花香气主要由芳樟醇、乙酸卞酯和α-法呢烯组成，由茉莉鲜花窨制形成的花茶中α-法呢烯的含量也很高。实验中的Y1和Y2号茶样均为玉兰打底茶样，其含有的α-法呢烯相对含量均在8％以上。因此，在研究茉莉花茶香气品质与香气成分相关性时，不考虑α-法呢烯香气成分的作用，以排除可能由玉兰香气成分带来的影响。
以茶叶检测所有香气成分为指标，利用MPP软件构建数据矩阵，进行主成分分析和聚类分析。主成分分析结果如图1所示，图中每一个点代表1个茶叶样本。前3个主成分贡献率分别为43.82％、23.53％和17.20％，其累积贡献率达84.55％，在PCA得分图中，11个茶叶样本分为4组，Y1、Y2和Y3号茶样分为1组，Y4、Y5、Y6和Y7号茶样分为1组，Y8和Y10号茶样分为1组；Y9和Y11号茶样分为1组。聚类分析结果和主成分分析一致。
利用SPSS软件对可鉴定的香气成分进行主成分分析，结果显示前7个主成分的特征根λ>1，这7个主成分的累计方差贡献率达到95.94％，这表明前7个主成分能够代表全部可鉴定的香气成分组成。通过计算得到各茶叶样本主成分综合得分如表3所示。11个茶样样品的品质高低排序分别是：Y11、Y10、Y7、Y8、Y9、Y4、Y5、Y6、Y3、Y1、Y2。
表3不同级别的福州茉莉花茶香气成分主成分分析
| 茶叶样本 | Y1 | Y2 | Y3 | Y4 | Y5 | Y6 | Y7 | Y8 | Y9 | Y10 | Y11 |
| 主成分综合得分 | -3.02 | -3.70 | -1.86 | 0.27 | -0.06 | -0.37 | 1.61 | 0.66 | 0.34 | 1.62 | 4.50 |
| 排名 | 10 | 11 | 9 | 6 | 7 | 8 | 3 | 4 | 5 | 2 | 1 |
2.3茉莉花茶香气成分评价指标的构建
主成分分析结果显示了可鉴定香气成分在各主成分上的载荷量分布，其中与主成分有较大正相关的成分包括：丙酸香叶酯、顺式-3-己烯醇苯甲酸酯、苯甲酸苄酯、吲哚、氨茴酸甲酯、大牛儿烯D、β-榄香烯、丁香烯、β-蒎烯、蛇麻烯、β-法呢烯、cis-Muurola-4(15),5-diene、γ-依兰油烯、δ-杜松烯、α-杜松烯和1,5,5-三甲基-6-亚甲基-环己烯；与主成分有较大负相关的香气成分包括：芳樟醇、乙酸叶醇酯、乙酸卞酯和β-环柠檬醛。
选择其中香气成分相对含量较高的组分，构建用以评价茉莉花茶香气品质的计算公式，即XFJTF＝(顺式-3-己烯醇苯甲酸酯+吲哚+氨茴酸甲酯)含量/(芳樟醇+乙酸叶醇酯+乙酸卞酯)含量×100，得分越高，花茶品质越好，价格越高。各茶叶的XFJTF得分计算结果如表4所示。
表4不同级别的福州茉莉花茶香气品质评价新指数
根据表4得分结果，可将不同级别的茉莉花茶品质分为0-15(低等)、16-30分(中等)、31-45分(高等)、46-60分(优等)，当香气得分高于61分，可定义为特优级茶叶。除Y7号茶样外，其他样本的得分高低与定价排序非常吻合。
2.4茉莉花茶香气品质评价指标的验证
以该公司生产的茶样(品名：松针；定价：190元/斤)进行验证，利用构建的香气品质评价得分(XFJTF)公式计算该验证茶样品质评价得分为25.46，位于Y3-Y5茶样之间，属于中等品质的茶，品质与定价范围相吻合。上述研究说明该指数能够较好的反应茉莉花茶的品质。
利用构建的香气品质评价得分评价市场随机抽取的茉莉花茶茶样，计算结果如表5所示。结果表明，利用XFJTF指数对市场随机抽样的花茶香气品质评价与专家审评得分基本一致。研究发现S3和S4样品的专家香气审评得分一样，计算的XFJTF指数数值相差极小，而JTF指数差异约1.5倍；S6样品的专家审评香气得分和XFJTF指数都略高于S5样品，但S5样品的JTF指数值为S6的1.7倍，这说明XFJTF指数评价花茶香气品质比JTF指数准确度和区分度更高。
表5市售茉莉花茶样本香气品质评价
| 市场随机茉莉花茶样 | S1 | S2 | S3 | S4 | S5 | S6 | S7 | S8 |
| 专家审评总得分 | 57.9 | 66.7 | 82.6 | 84.25 | 83.4 | 83.95 | 87.85 | 87.45 |
| 专家审评香气得分 | 50 | 58 | 78 | 78 | 83 | 84 | 85 | 88 |
| JTF指数 | 0.12 | 0.27 | 0.39 | 0.59 | 1.25 | 0.75 | 0.83 | 1.49 |
| XFJTF得分 | 5.58 | 9.26 | 13.91 | 14.33 | 17.85 | 18.30 | 26.23 | 41.81 |
进一步，以福州市茶王赛样本(售价>1万元)进行验证，计算得到的14个福州茉莉特种茶茶王赛样本得分均高于61分，为特优级茉莉花茶。不同形状的茉莉特种茶各自按照相应标准样进行专家审评得分，将本方法构建的香气品质评价得分顺序与专家审评得分进行对比发现，茉莉扁形茶、茉莉圆珠茶和茉莉条形茶等三种特种茶香气品质得分顺序与专家评审得分顺序一致；茉莉束形茶除1号样本外，另外2个茶样顺序一致；茉莉卷曲茶除3号样本外，另外两个茶样顺序一致。综上，XFJTF得分指数对14个福州茉莉特种茶茶王赛样本评价的准确度可以达到85.7％；而JTF指数对14个福州茉莉特种茶茶王赛样本评价的准确度仅为64.3％。这说明本方法建立的XFJTF得分指数对福州茉莉花茶香气品质评价更接近专家评审意见。
表6福州茉莉花茶王赛茶样本香气品质评价
综上，花茶的香气质量是评价茉莉花茶品质的重要指标。本发明筛选出对主成分有显著影响的香气成分，构建了香气品质评价得分公式：XFJTF＝(顺式-3-己烯醇苯甲酸酯+吲哚+氨茴酸甲酯)含量/(芳樟醇+乙酸叶醇酯+乙酸卞酯)含量×100，根据得分将花茶分为5个级别(低等、中等、高等、优级、特优级)，得分越高，香气品质越好，价格越贵。利用该XFJTF得分指数对茉莉花茶评价的准确度可以达到85.7％，比Lin等提出的JTF评价指数的准确度提高了约20％。本方法不受主观因素的影响，能够做到标准化评价，评判结果客观、可行，能够真实区分茉莉花茶品质的优劣。本发明建立的花茶香气品质评价指标，有效增强了茉莉花茶生产和品质评价的科学性，为研究茉莉花茶质量标准体系研究提供科学依据。
需要说明的是，尽管在本文中已经对上述各实施例进行了描述，但并非因此限制本发明的专利保护范围。因此，基于本发明的创新理念，对本文所述实施例进行的变更和修改，或利用本发明说明书及附图内容所作的等效结构或等效流程变换，直接或间接地将以上技术方案运用在其他相关的技术领域，均包括在本发明的专利保护范围之内。
Claims (7)
1.一种茉莉花茶香气品质评价方法，其特征在于：所述的评价方法是根据(顺式-3-己烯醇苯甲酸酯+吲哚+氨茴酸甲酯)含量/(芳樟醇+乙酸叶醇酯+乙酸卞酯)含量，这一比值的大小判断茉莉花茶的品质。
2.根据权利要求1所述的茉莉花茶香气品质评价方法，其特征在于：包括如下步骤：
采用顶空固相微萃取方法富集花茶香气成分；
利用GC-MS技术测定茉莉花茶香气组成；
构建茉莉花茶香气品质的计算公式，即XFJTF得分＝(顺式-3-己烯醇苯甲酸酯+吲哚+氨茴酸甲酯)含量/(芳樟醇+乙酸叶醇酯+乙酸卞酯)含量×100；
根据茉莉花茶香气得分判断茉莉花茶的品质，将不同级别的茉莉花茶品质分为：低等，得分0-15分；中等，得分16-30分；高等，得分31-45分；优等，得分46-60分；特优等，得分≥61分。
3.根据权利要求2所述的茉莉花茶香气品质评价方法，其特征在于：所述的顶空固相微萃取方法包括如下步骤：
萃取头老化：萃取头用丙酮浸泡20-40min后，65μm聚二甲基硅氧烷/二乙烯基苯萃取头在240-260℃老化20-40min；
萃取条件：称取1-2g茶叶置于密封的顶空瓶中，60-70℃水浴5-10min后插入SPME纤维头吸附15-25min，240-260℃解吸3-5min。
4.根据权利要求2所述的茉莉花茶香气品质评价方法，其特征在于：所述的GC-MS技术测定茉莉花茶香气组成的方法如下：
色谱条件：进样口温度240-260℃，柱温40-60℃；程序为：起始温度40-60℃，保持2-3min，以4-5℃/min升到120-130℃，保持15-20min，以4-5℃/min升到170-180℃，保持2-3min，以30-40℃/min升到280-290℃，保持2-3min；
质谱条件：离子源EI；采集模式为全扫描；溶剂延迟5-8min；EMV模式为相对值；质量扫描范围：25.00～550.00amu；MS离子源温度为220-240℃，MS四级杆温度140-160℃；
检测的化合物经谱库检索，同时采用线性升温公式计算各组分的实验保留指数，结合文献进行花茶香气成分鉴定；香气组分相对含量采用峰面积归一化法进行计算，表示为各香气组分的峰面积占总峰面积之比值。
5.根据权利要求2所述的茉莉花茶香气品质评价方法，其特征在于：所述的香气成分包括醇类、酯类、含氮化合物和萜烯类化合物；其中，醇类化合物以芳樟醇和苯甲醇为主，酯类化合物以乙酸卞酯、乙酸叶醇酯、顺式-3-己烯醇苯甲酸酯和水杨酸甲酯为主，含氮化合物以吲哚和氨茴酸甲酯为主，萜烯类化合物以α-法呢烯为主。
6.一种如权利要求1-5中任一所述的茉莉花茶香气品质评价方法在福州茉莉花茶品质评价中的应用。
7.一种如权利要求1-5中任一所述的茉莉花茶香气品质评价方法在茉莉扁形茶或茉莉圆珠茶或茉莉条形茶品质评价中的应用。
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