CN102680427A - Method for identifying cigarette surface aroma quality by applying near infrared spectrum analysis technology - Google Patents
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Abstract
本发明公开了一种应用近红外光谱分析技术鉴别卷烟表香质量的方法。首先将合格表香的光谱数据存入计算机,应用TQ analyst7.1软件中的相似度匹配的定性分析方法建立该品牌表香的相似度匹配模型,经计算得到该品牌表香的相似度匹配临界值。在鉴别表香质量时,应用同样方法采集待鉴别表香的光谱数据,并计算待鉴别表香的光谱相似度匹配值,当待鉴别表香的相似度匹配值≥该品牌卷烟表香的相似度匹配临界值时鉴定为合格,否则即为不合格。该鉴别方法所需样品量较少,鉴别过程无需前处理及制样程序,鉴别过程简单,非常适合在烟草行业进行推广,在卷烟表香质量稳定性控制中具有良好的应用前景。The invention discloses a method for identifying the quality of cigarette surface aroma by applying near-infrared spectrum analysis technology. Firstly, the spectral data of qualified table fragrances are stored in the computer, and the similarity matching model of the brand table fragrances is established by using the qualitative analysis method of similarity matching in TQ analyst7.1 software, and the similarity matching criticality of the brand table fragrances is obtained through calculation. value. When identifying the quality of the surface aroma, apply the same method to collect the spectral data of the surface aroma to be identified, and calculate the spectral similarity matching value of the surface aroma to be identified, when the similarity matching value of the surface aroma to be identified ≥ the similarity It is qualified when the degree matches the critical value, otherwise it is unqualified. The identification method requires less samples, and the identification process does not require pretreatment and sample preparation procedures. The identification process is simple, and it is very suitable for promotion in the tobacco industry, and has a good application prospect in the quality stability control of cigarette flavor.
Description
技术领域 technical field
本发明属于卷烟质量控制技术领域,具体涉及一种应用近红外(NIR)光谱分析技术鉴别卷烟表香质量的方法。 The invention belongs to the technical field of cigarette quality control, and in particular relates to a method for identifying the quality of cigarette surface aroma by applying near-infrared (NIR) spectral analysis technology. the
背景技术 Background technique
卷烟加香的目的主要是用以衬托烟香,在不损害烟叶原有香气的前提下掩盖杂气。由于叶组质量的差异及降焦措施的运用,会导致卷烟产品香气缺乏或滞重,通过加香可以补充优美的香气;加香还可以添加挥发性较强的特征香料,赋予卷烟独特的香味,增加对消费者的吸引力;此外,加香还能够增加甜润感、改善吸味,掩盖或减弱一些杂气、刺激性、干燥感和粗糙感;加香更重要的作用是能把不同类型、不同品种、不同产地、不同年份生产的不同等级烟叶的香气有机组合并协调起来,同时还能掩盖或冲淡杂气,改善品质。因此,卷烟表香的质量稳定性直接关系到卷烟产品的质量稳定性。而烟用表香大多取材于天然香料,受到原料、加工等多种因素的影响,其化学成分的复杂性和多样性一直都是质量控制的重点和难点。 The purpose of cigarette flavoring is mainly to set off the aroma of cigarettes and cover up miscellaneous odors without damaging the original aroma of tobacco leaves. Due to the difference in the quality of the leaves and the application of coke reduction measures, the aroma of cigarette products will be lacking or sluggish. Flavoring can supplement the beautiful aroma; flavoring can also add highly volatile characteristic spices to give cigarettes a unique aroma , to increase the appeal to consumers; in addition, flavoring can also increase the sweetness, improve the taste, cover up or weaken some miscellaneous, irritating, dry and rough; the more important role of flavoring is to make different types of The aromas of different grades of tobacco leaves produced in different varieties, different origins, and different years are organically combined and coordinated, and at the same time, it can cover up or dilute the miscellaneous odors and improve the quality. Therefore, the quality stability of cigarette top flavor is directly related to the quality stability of cigarette products. The surface flavors for tobacco are mostly made of natural spices, which are affected by various factors such as raw materials and processing. The complexity and diversity of its chemical components have always been the focus and difficulty of quality control. the
现有卷烟表香的质量控制方法主要是通过酸度、混溶度、折光指数、挥发分总量和旋光度等物性指标和调香师的人工嗅香等,方法较为单一和片面。运用色谱指纹图谱的方法对卷烟香精香料进行质量控制是目前研究的热点,但色谱分析技术前处理过程繁杂,限制了色谱指纹图谱的应用。因此,为了保证来自不同原料产地和不同批次的卷烟表香质量的一致性,迫切要求 开发一种更优化的卷烟表香质量鉴别方法。近红外光谱分析技术是近年来迅速发展起来的一种方便、高效、低成本的绿色分析技术,目前已经广泛应用于农业、林业、造纸、茶叶、食品、中草药鉴别等行业,但该方法在卷烟表香质量鉴别方面的应用尚未见报道。 The existing quality control methods for cigarette surface aroma are mainly based on physical indicators such as acidity, miscibility, refractive index, total volatile matter, optical rotation, etc., and manual smelling by perfumers. The method is relatively single and one-sided. The use of chromatographic fingerprints to control the quality of cigarette flavors and fragrances is a research hotspot at present, but the pretreatment process of chromatographic analysis technology is complicated, which limits the application of chromatographic fingerprints. Therefore, in order to ensure the consistency of the quality of cigarette flavors from different raw material origins and different batches, it is urgent to develop a more optimized method for identifying the quality of cigarette flavors. Near-infrared spectral analysis technology is a convenient, efficient and low-cost green analysis technology developed rapidly in recent years. It has been widely used in industries such as agriculture, forestry, papermaking, tea, food, and Chinese herbal medicine. The application of the quality identification of surface aroma has not been reported yet. the
发明内容 Contents of the invention
本发明的目的在于针对现有的不足,提供一种应用近红外光谱分析技术鉴别卷烟表香质量的方法。利用FT-NIR光谱数据,应用相似度匹配的定性分析方法直接建立卷烟表香质量控制模型,实现对卷烟表香质量的快速、精确地鉴别。 The purpose of the present invention is to provide a method for identifying the quality of cigarette surface aroma by applying near-infrared spectrum analysis technology to address the existing deficiencies. Using FT-NIR spectral data, the qualitative analysis method of similarity matching is used to directly establish the quality control model of cigarette flavor, so as to realize the rapid and accurate identification of the quality of cigarette flavor. the
本发明的目的通过以下技术方案予以实现。 The purpose of the present invention is achieved through the following technical solutions. the
除非另有说明,本发明所采用的百分数均为重量百分数。 Unless otherwise stated, the percentages used in the present invention are all percentages by weight. the
一种应用近红外光谱分析技术鉴别卷烟表香质量的方法,包括以下步骤: A method for identifying the quality of cigarette surface aroma by using near-infrared spectral analysis technology, comprising the following steps:
(1)光谱数据采集:将某品牌卷烟合格的表香样品装入小试管中,置于透射样品架上采集表香样品的近红外透射光谱数据,每个样品进行10次重复数据采集,并将所采集的光谱数据存入计算机;光谱采集方式为:透射光谱采集模式;扫描范围:4000~10000cm-1;分辨率:8 cm-1;扫描次数:16次;每次采集样品光谱前均须采集背景光谱; (1) Spectral data collection: Put the qualified surface aroma samples of a certain brand of cigarettes into small test tubes, place them on the transmission sample rack to collect the near-infrared transmission spectrum data of the surface aroma samples, and repeat the data collection 10 times for each sample, and Store the collected spectral data into the computer; the spectral collection method is: transmission spectrum collection mode; scanning range: 4000-10000 cm -1 ; resolution: 8 cm -1 ; scanning times: 16 times; A background spectrum must be collected;
(2)模型构建:应用TQ analyst7.1软件中的相似度匹配的定性分析方法建立该卷烟品牌表香的相似度匹配模型; (2) Model construction: Apply the qualitative analysis method of similarity matching in TQ analyst7.1 software to establish the similarity matching model of the cigarette brand's surface flavor;
(3)相似度匹配临界值计算:以相似度匹配模型为基础,运用TQ analyst7.1软件计算该品牌卷烟表香的光谱相似度匹配值(Similarity Match Value, SMV),并对该品牌卷烟表香的SMV值进行统计分析,分析SMV数据分布的范围,确定SMV的最下限数值Min;同样地,批量采集同一企业生产的非该品牌卷烟表香的光谱数据,并对非该品牌卷烟表香的SMV值进行计算,对所得到的SMV值进行统计分析,分析SMV数据分布的范围,确定SMV的最上限数值Max;经计算得到该品牌卷烟表香的相似度匹配临界值CV: (3) Calculation of similarity matching threshold value: Based on the similarity matching model, use TQ analyst7.1 software to calculate the spectral similarity matching value (Similarity Match Value, SMV) of the brand's cigarette surface flavor, and the brand's cigarette table flavor Statistically analyze the SMV value of cigarettes, analyze the range of SMV data distribution, and determine the minimum value Min of SMV; similarly, collect the spectral data of non-brand cigarettes produced by the same enterprise in batches, and analyze the non-brand cigarettes. Calculate the SMV value of the cigarette, conduct statistical analysis on the obtained SMV value, analyze the distribution range of SMV data, and determine the upper limit value Max of SMV; the similarity matching critical value CV of the brand's cigarette surface fragrance is obtained through calculation:
CV=(Min+ Max)/2 CV=(Min+Max)/2
(4)鉴别:重复步骤(1),采集待鉴别卷烟表香的光谱数据,以该品牌卷烟表香的相似度匹配模型为基础,通过TQ analyst7.1软件计算待鉴别卷烟表香的SMV,当待鉴别卷烟表香的SMV≥CV时鉴定为该表香质量合格,否则为不合格。 (4) Identification: Repeat step (1) to collect the spectral data of the surface flavor of the cigarette to be identified, and calculate the SMV of the surface flavor of the cigarette to be identified by TQ analyst7.1 software based on the similarity matching model of the brand’s cigarette surface flavor. When the SMV ≥ CV of the surface flavor of the cigarette to be identified is identified as qualified, otherwise it is unqualified. the
步骤(1)所述的合格表香样品为该品牌不同时间、不同批次生产的合格样品。 The qualified surface fragrance samples mentioned in step (1) are qualified samples produced by the brand at different times and in different batches. the
与现有技术相比,本发明具有如下优点: Compared with prior art, the present invention has following advantage:
1、应用现有近红外光谱分析仪器,结合TQ analyst光谱分析软件中相似度匹配的光谱数据定性分析功能,非常简单地建立鉴别模型。 1. Using the existing near-infrared spectral analysis instrument, combined with the qualitative analysis function of spectral data similarity matching in the TQ analyst spectral analysis software, it is very simple to establish an identification model. the
2、鉴别过程简单,模型建好后,无需专业背景人员即可完成鉴别过程,易于推广。 2. The identification process is simple. After the model is built, the identification process can be completed without professional background personnel, which is easy to promote.
3、模型鉴别效果检验表明,模型鉴别准确率较高,可以作为一种有效的卷烟表香质量稳定性评价和检测工具。 3. The test of model identification results shows that the accuracy of model identification is high, and it can be used as an effective evaluation and detection tool for quality stability of cigarette flavor. the
具体实施方式 Detailed ways
下面通过应用实施例对本发明作进一步的详细说明,但实施例并不是对本发明技术方案的限定。 The present invention will be further described in detail through application examples below, but the examples do not limit the technical solution of the present invention. the
应用实施例1 Application Example 1
应用近红外光谱分析技术无损鉴别云烟(软珍品)表香的质量。 The quality of surface fragrance of Yunyan (soft treasure) is non-destructively identified by near-infrared spectral analysis technology. the
1、样品准备:准备红云红河烟草(集团)有限责任公司昆明卷烟厂配料中心生产的云烟(软珍品)的合格表香样品20批,每批取100克用于模型的构建。 1. Sample preparation: prepare 20 batches of qualified surface aroma samples of Yunyan (soft treasure) produced by the ingredient center of Kunming Cigarette Factory of Hongyun Honghe Tobacco (Group) Co., Ltd., and take 100 grams from each batch for the construction of the model. the
2、光谱数据采集:应用热电公司的Nicolet Antaris型FT-近红外光谱仪对样品进行光谱采集。光谱采集之前,开机预热FT-NIR光谱仪2小时。分别将不同表香样品装入小试管中,置于透射样品架上采集表香样品的近红外透射光谱数据。每个样品进行10次重复数据采集,并将所采集的光谱数据存入计算机;其中光谱采集方式为:透射光谱采集模式;扫描范围(Data Range):4000~10000cm-1;分辨率(Resolution):8 cm-1;扫描次数:16次;每次采集样品光谱前均须采集背景光谱。 2. Spectral data acquisition: The Nicolet Antaris FT-near-infrared spectrometer of Thermoelectric Company was used to collect the spectrum of the sample. Before spectrum collection, turn on the FT-NIR spectrometer to warm up for 2 hours. Put different surface fragrance samples into small test tubes, and place them on the transmission sample holder to collect the near-infrared transmission spectrum data of the surface fragrance samples. Data collection was repeated 10 times for each sample, and the collected spectral data was stored in the computer; the spectral collection method was: transmission spectrum collection mode; scanning range (Data Range): 4000~10000cm -1 ; resolution (Resolution) : 8 cm -1 ; number of scans: 16 times; the background spectrum must be collected before each sample spectrum is collected.
3、模型构建: 3. Model construction:
为了减小由于样品均匀性等因素对光谱带来的多重偏差,应用TQ analyst7.1软件中的附加散射校正技术(Multiplicative Scatter Correction, MSC)对原始FT-NIR光谱进行处理。同时,建立模型时对相关参数进行调整和优化是提高模型预测能力和预测效果的主要手段之一。对光谱进行平滑处理和基线校正,能有效去除近红外光谱信号中的基线漂移与光散射等各种干扰和噪声,充分提取FT-NIR光谱包含的有效特征信息,提高模型的预测精度。另外,选择恰当的光谱范围也是建模过程中一个重要的环节之一。通过对模型的多次优化计算,选择恰当参数建立云烟(软珍品)卷烟表香的相似度匹配(Similarity Match)模型。表1为云烟(软珍品)卷烟表香的建模参数设置。 In order to reduce the multiple deviations caused by factors such as sample uniformity, the original FT-NIR spectrum was processed with the additional scatter correction technology (Multiplicative Scatter Correction, MSC) in TQ analyst7.1 software. At the same time, adjusting and optimizing relevant parameters when building a model is one of the main means to improve the predictive ability and effect of the model. Smoothing and baseline correction of the spectrum can effectively remove various interferences and noises such as baseline drift and light scattering in the near-infrared spectrum signal, fully extract the effective feature information contained in the FT-NIR spectrum, and improve the prediction accuracy of the model. In addition, choosing an appropriate spectral range is also one of the important links in the modeling process. Through multiple optimization calculations on the model, appropriate parameters were selected to establish a Similarity Match model for the surface aroma of Yunyan (soft treasure) cigarettes. Table 1 shows the modeling parameter settings of Yunyan (soft treasure) cigarette flavor. the
表1 云烟(软珍品)表香相似度匹配模型的建模优化参数 Table 1 The modeling optimization parameters of the similarity matching model of Yunyan (soft treasures)
4、计算相似度匹配临界值: 4. Calculate the similarity matching threshold:
以云烟(软珍品)表香的相似度匹配模型为基础,运用TQ analyst7.1软件计算云烟(软珍品)表香的SMV,并对所得到的SMV值进行统计分析,分析SMV数据分布的范围,确定SMV的最下限数值Min为94.12;同样地,批量采集非云烟(软珍品)表香的光谱数据,对非云烟(软珍品)表香的SMV进行相应的计算,并对所得到的SMV进行统计分析,分析SMV数据分布的范围,确定SMV的最上限数值Max为78.17;经计算得到云烟(软珍品)表香的相似度匹配临界值CV=(94.12+78.17)/2=86.15。 Based on the similarity matching model of Yunyan (soft treasure) surface fragrance, use TQ analyst7.1 software to calculate the SMV of Yunyan (soft treasure) surface fragrance, and conduct statistical analysis on the obtained SMV value, and analyze the distribution range of SMV data , determine the minimum value Min of SMV as 94.12; similarly, collect the spectral data of non-yunyan (soft treasures) surface fragrance in batches, calculate the SMV of non-yunyan (soft treasures) surface fragrance, and calculate the obtained SMV Statistical analysis was carried out to analyze the distribution range of SMV data, and the upper limit value Max of SMV was determined to be 78.17; the similarity matching critical value of Yunyan (soft treasure) surface fragrance was obtained by calculation CV=(94.12+78.17)/2=86.15. the
5、鉴别:重复步骤2,采集待鉴别表香的光谱数据,以云烟(软珍品)表香的相似度匹配模型为基础,通过TQ analyst7.1软件计算待鉴别表香的SMV,当待鉴别表香的SMV≥86.15时鉴定为云烟(软珍品)的合格表香,否则即为不合格。 5. Identification: Repeat step 2 to collect the spectral data of the surface fragrance to be identified. Based on the similarity matching model of Yunyan (soft treasure) surface fragrance, calculate the SMV of the surface fragrance to be identified by TQ analyst7.1 software. When the SMV of the surface incense is ≥ 86.15, it is identified as a qualified surface incense of Yunyan (soft treasure), otherwise it is unqualified. the
应用实施例2 Application Example 2
应用近红外光谱分析技术无损鉴别云烟(紫)表香的质量: Non-destructive identification of the quality of Yunyan (purple) table fragrance by using near-infrared spectral analysis technology:
1、样品准备:样品用云烟(紫)表香,其它同实施例1。 1. Sample preparation: use Yunyan (purple) surface fragrance for the sample, and the others are the same as in Example 1. the
2、光谱数据采集:同实施例1。 2. Spectral data collection: same as in Example 1. the
3、模型构建:所选择的建模参数如表2,其它同实施例1。 3. Model construction: the selected modeling parameters are shown in Table 2, and others are the same as in Example 1. the
表2 云烟(紫)表香相似度匹配模型的建模优化参数 Table 2 The modeling optimization parameters of the similarity matching model of Yunyan (purple) fragrance
4、计算相似度匹配临界值:以云烟(紫)表香的相似度匹配模型为基础,计算得到云烟(紫)表香的相似度匹配临界值CV=(97.07+77.94)/2=87.51。 4. Calculate the similarity matching critical value: Based on the similarity matching model of Yunyan (purple) superficial incense, calculate the similarity matching critical value of Yunyan (purple) superficial incense CV=(97.07+77.94)/2=87.51. the
5、鉴别:重复步骤2,采集待鉴别表香的光谱数据,以云烟(紫)表香的相似度匹配模型为基础,通过TQ analyst7.1软件计算待鉴别表香的SMV,当待鉴别表香的SMV≥87.51时鉴定为云烟(紫)的合格表香,否则即为不合格。 5. Identification: Repeat step 2 to collect the spectral data of the table fragrance to be identified. Based on the similarity matching model of Yunyan (purple) table fragrance, calculate the SMV of the table fragrance to be identified by TQ analyst7.1 software. When the table fragrance to be identified When the SMV of the incense is ≥ 87.51, it is identified as a qualified surface incense of Yunyan (purple), otherwise it is unqualified. the
应用实施例3 Application Example 3
应用近红外光谱分析技术无损鉴别云烟(红)卷烟的真伪: Non-destructive identification of the authenticity of Yunyan (red) cigarettes by using near-infrared spectroscopy analysis technology:
1、样品准备:样品用云烟(红),其它同实施例1。 1. Sample preparation: Yunyan (red) is used as the sample, and the others are the same as in Example 1. the
2、光谱数据采集:同实施例1。 2. Spectral data collection: same as in Example 1. the
3、模型构建:所选择的建模参数如表3,其它同实施例1。 3. Model construction: the selected modeling parameters are shown in Table 3, and others are the same as in Example 1. the
表3 云烟(红)表香相似度匹配模型的建模优化参数 Table 3 The modeling optimization parameters of the similarity matching model of Yunyan (red) table fragrance
4、计算相似度匹配临界值:以云烟(红)表香的相似度匹配模型为基础,计算得到云烟(红)表香的相似度匹配临界值CV=(96.08+79.60)/2=87.84。 4. Calculation of similarity matching critical value: Based on the similarity matching model of Yunyan (red) surface incense, calculate the similarity matching critical value of Yunyan (red) surface incense CV=(96.08+79.60)/2=87.84. the
5、鉴别:重复步骤2,采集待鉴别表香的光谱数据,以云烟(红)表香的相似度匹配模型为基础,通过TQ analyst7.1软件计算待鉴别表香的SMV,当待鉴别表香的SMV≥87.84时鉴定为云烟(红)的合格表香,否则即为不合格。 5. Identification: Repeat step 2 to collect the spectral data of the table fragrance to be identified, and use the TQ analyst7.1 software to calculate the SMV of the table fragrance to be identified based on the similarity matching model of Yunyan (red) table fragrance. When the SMV of the incense is ≥ 87.84, it is identified as a qualified table incense of Yunyan (red), otherwise it is unqualified. the
应用实施例4 Application Example 4
对云烟(软珍品)、云烟(紫)和云烟(红)3个牌号卷烟的表香进行鉴别,考察该方法的鉴别准确率。分别取30个表香样品(其中20个为模型校正集牌号表香,10个为非模型校正集牌号表香)进行鉴定,分别得到每个样品与校正集样品的SMV。结果见表4,5和6。结果表明,它们对卷烟表香的 质量鉴别判断能力均达到100%。 The surface aroma of Yunyan (soft treasure), Yunyan (purple) and Yunyan (red) cigarettes were identified, and the identification accuracy of the method was investigated. Take 30 surface fragrance samples (20 of which are brand surface fragrances in the model calibration set, and 10 are non-model calibration set brand surface fragrances) for identification, and obtain the SMV of each sample and the sample in the calibration set. The results are shown in Tables 4, 5 and 6. The results showed that their ability to identify and judge the quality of cigarette surface flavors all reached 100%. the
表4 云烟(软珍品)表香相似度匹配模型对不同类型表香的预测结果 Table 4 The prediction results of Yunyan (soft treasure) surface aroma similarity matching model for different types of surface aroma
表5 云烟(紫)表香相似度匹配模型对不同类型表香的预测结果 Table 5 Prediction results of Yunyan (purple) superficial fragrance similarity matching model for different types of superficial fragrance
表6 云烟(红)表香相似度匹配模型对不同类型表香的预测结果 Table 6 The prediction results of Yunyan (red) surface aroma similarity matching model for different types of surface aroma
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