CN105092516A - Digital light processing technology-based portable liquid food near infrared spectroscopy analyzer - Google Patents

Digital light processing technology-based portable liquid food near infrared spectroscopy analyzer Download PDF

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CN105092516A
CN105092516A CN 201410576952 CN201410576952A CN105092516A CN 105092516 A CN105092516 A CN 105092516A CN 201410576952 CN201410576952 CN 201410576952 CN 201410576952 A CN201410576952 A CN 201410576952A CN 105092516 A CN105092516 A CN 105092516A
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sample
preservative
light source
infrared spectroscopy
near infrared
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CN 201410576952
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冯海涛
施光典
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深圳莱特光电有限公司
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Abstract

The invention discloses a digital light processing technology-based portable liquid food near infrared spectroscopy analyzer. The digital light processing technology-based portable liquid food near infrared spectroscopy analyzer comprises a LED light source assembly, a reflective mirror/condensing lens, a blazed grating, a digital micromirror assembly, a single-photon detector, a linear detector and a spectral information processing system. The near infrared spectroscopy analyzer utilizes a matrix composed of multiple LED chips as a near infrared spectroscopy analyzer light source. The condensing lens is arranged at the outer side of the LED chip so that a light source luminescence area is reduced and enough light source intensity is provided. The LED chip has the characteristics of high light intensity and low power and is conducive to reduction of a near infrared spectroscopy analyzer volume so that the near infrared spectroscopy analyzer is portable and is suitable for fluid food detection.

Description

一种基于数字光处理技术的便携式液体食物近红外光谱分析仪 Based portable digital light processing liquid food technology Near Infrared Analyzer

技术领域 FIELD

[0001] 本发明涉及食品添加剂检测技术领域,具体涉及一种基于数字光处理技术的便携式液体食物近红外光谱分析仪。 [0001] The present invention relates to the technical field of detection of food additives, particularly liquid food to a portable digital light processing technology based on near-infrared spectroscopy.

背景技术 Background technique

[0002] 防腐剂是各种流体食物(如果汁、酒、乳制品)中常用的食品添加剂,可有效延长含水量较高的流体食物的保质期。 [0002] Food preservatives of various fluids (such as fruit juice, wine, dairy products) commonly used food additive, can effectively extend the shelf life of the high water content of the fluid food. 其中苯甲酸类防腐剂在国内食品加工业中尤为常见。 Benzoate preservatives in the country in which the food processing industry is particularly common. 流体食物中过量的苯甲酸类防腐剂容易引发严重过的中毒现象,因此,苯甲酸含量是食品检测中一个重要的检测项目。 Excess fluid food preservatives benzoic acid is apt to cause serious poisoning had, therefore, benzoic acid content of food testing is an important test items. 现常用近红外光谱仪检测食物中防腐剂的含量。 Now commonly used by near infrared spectroscopy to detect food preservatives.

[0003] 近红外光(Near Infrared,NIR)是介于可见光(VIS)和中红外(MIR)之间的电磁辐射波,美国材料检测协会(ASTM)将近红外光谱区定义为780~2526nm的区域,是人们在吸收光谱中发现的第一个非可见光区。 [0003] NIR (Near Infrared, NIR) is electromagnetic radiation between visible light (VIS) and infrared (MIR) between a defined area near-infrared spectrum of the American Society for Testing Materials (ASTM) as a region of 780 ~ 2526nm , a first non-visible region has been found in the absorption spectrum. 近红外光谱区与有机分子中含氢基团(〇H、NH、CH) 振动的合频和各级倍频的吸收区一致,通过扫描样品的近红外光谱,可以得到样品中有机分子含氢基团的特征信息,而且利用近红外光谱技术分析样品具有方便、快速、高效、准确和成本较低,不破坏样品,不消耗化学试剂,不污染环境等优点,近红外光谱仪已广泛应用于农产业、石化产品、临床诊断、环境检测等领域。 Near infrared spectral regions and hydrogen-containing organic group in the molecule (〇H, NH, CH) consistent with engagement of vibration frequency and the frequency levels of the absorption zone, by near-infrared spectral scan of the sample, the sample can be obtained a hydrogen-containing organic molecules wherein the group information, and the use of near infrared spectroscopy analysis of a sample having a convenient, fast, efficient, accurate and low cost, does not destroy the sample does not consume chemical reagents, no environmental pollution, etc., near-infrared spectroscopy has been widely used in agriculture industrial, petrochemical products, clinical diagnostics, environmental testing and other areas.

[0004] 在食品工业中,近红外光谱仪很多时候用于携带到现场进行分析,因此需要体积小巧、方便携带的近红外光谱仪,现有的便携式近红外光谱仪的种类有很多,根据光路结构不同可分为:滤光片型、光栅型、傅里叶变换型、基于数字微镜元件(DMD)的微机电系统(MEMS)型。 [0004] In the food industry, near infrared spectrometer often used to carry to the scene analysis, it is necessary compact, portable NIR spectrometer, a conventional portable near-type infrared spectrometer has a lot, depending on the optical structure may be divided into: filter type, grating, Fourier transform, based on the digital micromirror device (DMD) microelectromechanical system (MEMS) type.

[0005] Zeltex公司的ZX-50系列手持式近红外粮食分析仪是滤光片型的典型代表,其缺点是波长数目有限,准确度和精度不高。 [0005] Zeltex's ZX-50 Series handheld grain near-infrared analyzer is a typical representative of type filter, which disadvantage is the limited number of wavelengths, the accuracy and precision is not high.

[0006] 南京中地仪器的ZDJIPB-I近红外光谱仪是光栅扫描型光谱仪的典型代表,但因有移动部件导致仪器的抗震性差,扫描速度相对较慢。 [0006] Nanjing ZDJIPB-I to the instrument near infrared spectrometer is typical raster scanning spectrometer, has moving parts but result in seismic instrumentation differential scanning speed is relatively slow.

[0007] 傅里叶变换型光谱仪的光通量大、分辨率高,但抗震性差,很难做成便携式仪器。 [0007] Fourier Transform Spectrometer large luminous flux, high resolution, but poor shock, it is difficult to make the portable instrument.

[0008] DLP是"Digital Light Procession"的缩写,B卩为数字光处理,也就是说这种技术要先把影像信号经过数字处理,然后再把光投影出来。 [0008] DLP is an abbreviation for "Digital Light Procession" A, B Jie digital light processing, that is the technology for digitally processing a video signal first, and then the light is projected. 它是基于TI (美国德州仪器)公司开发的数字微镜元件-DMD (Digital Micromirror Device)来完成可视数字信息显示的技术。 It is TI (Texas Instruments) developed DMD -DMD (Digital Micromirror Device) technology to complete the visual display based on the digital information. 使用数字微镜元件(DMD)进行光谱选择的仪器以低成本的数字微镜元件(DMD)芯片和单点探测器代替光栅阵列型光谱仪中的线阵列探测器,成本大为降低,仪器结构简单, 制作容易,以不同的组合(阿达玛模板)选通多列微镜实现阿达玛变换,信噪比较不使用变换大大提升。 Using a digital micromirror device (DMD) for spectral selection of low-cost instrument digital micromirror device (DMD) chip and a single point detector line array detector instead of the array type grating spectrometer, greatly reduced cost, a simple apparatus structure , easy to manufacture, in different combinations (Hadamard template) micromirrors to achieve multi-column strobe Hadamard transform, using the transformation SNR less greatly enhanced. 波长精度〇. 6nm,仪器经过各种工业现场试验,稳定性较好,但是受单个探测器性能的限制,其对微弱光谱的探测能力有限。 Wavelength accuracy billion. Of 6 nm, through a variety of industrial field test instruments, good stability, but is limited by the performance of a single detector, its limited ability to detect faint spectrum. 为解决这一问题,申请号为2014101058442 的中国发明专利申请提供了一种近红外光谱仪,包括光源、抛物面反射镜、闪耀光栅、数字微镜器件、线性探测器、单光子探测器、光谱信息处理系统;所述光源设置在抛物面反射镜的焦点处,光源经抛物面反射镜准直后投射样品中,未被吸收的光经闪耀光栅在一级闪耀角上分开成单色平行光投射到数字微镜器件上;数字微镜器件中的微镜产生+ 12°和一12°的偏转,将单色平行光分别反射到线性探测器和单光子探测器上;光谱信息处理系统对线性探测器和单光子探测器接收的光谱信息进行融合、阿达玛变换处理,得到原始光谱信号的光谱强度。 To solve this problem, the Chinese Application No. 2014101058442 patent application provides a near-infrared spectrometer including a light source, a parabolic reflector, blazed grating, a digital micromirror device, linear detector, single-photon detector, the spectral information processing the system; the light source is disposed at the focal point of the parabolic mirror, the light source is projected by the parabolic mirror collimator sample after the unabsorbed light is separated into monochromatic parallel blazed grating light onto a digital micromirror on the blaze angle the mirror device; a digital micromirror device the mirrors in generating + 12 ° and a deflection of 12 °, are reflected monochromatic parallel light onto a linear detector and a single photon detector; spectral information processing system and linear detector spectral information received single-photon detector integration, processing the Hadamard transform, the spectral intensity of the original signal to obtain the spectrum. 为提高检测精度,其光源需为点光源,但受限于检测仪的体积,现有的点光源强度难以满足流体食物检测的需求(因流体食物浊度较高,且常悬浮用果胶、蛋白质等高分子物质,将干扰光线在样品中的传递,使光线减弱,进而使进入闪耀光栅的光信号强度不足)。 In order to improve the detection accuracy, it must be a point light source, but is limited by the volume of the detector, the strength of conventional point light sources is difficult to meet the demand of fluid food testing (due to high turbidity of the fluid food, and often suspended pectin, polymer substances such as proteins, to interfere with the transmission of light in the sample, so that light is reduced, thereby enabling the optical signal enters the blazed grating insufficient strength). 矩阵式LED能耗低而可以被制作为较小的体积,且足够多的LED可以提供满足测试需求的光强。 Low power consumption and LED matrix may be made as a smaller volume, and an LED can provide sufficient light intensity to meet testing needs. 但过多的LED芯片组成的光源其面积较大,无法形成点光源。 However, too much light LED chips whose area is larger, can not form a point light source. 采用可作为点光源的激光发生器作为光源时,其较高的耗能以及智能产生单色光的性质将使近红外光谱仪体积无法得到控制。 May be employed as the point light source as a light source a laser generator which generates a high energy monochromatic nature and intelligent near-infrared spectrometer will not be a volume control.

[0009] 如何克服上述现有技术的不足已成为现有光电分析领域亟待解决的重点难题。 Inadequate [0009] how to overcome the above-mentioned prior art problems have become the focus of analysis of existing photovoltaic field to be solved.

发明内容 SUMMARY

[0010] 有鉴于此,本发明公开一种高精度、便携的近红外光谱仪。 [0010] Accordingly, the present invention discloses a high-precision, portable near infrared spectrometer.

[0011] 本发明的目的通过以下技术方案实现: 一种基于数字光处理技术的便携式液体食物近红外光谱分析仪,包括LED光源组件、 反光镜、闪耀光栅、数字微镜组件、单光子探测器、线性探测器以及光谱信息处理系统,所述光谱信息处理系统与所述数字微镜组件、单光子探测器、线性探测器通信连接;所述LED光源组件包括散热基板、覆盖在散热基板上的线路板以及安装于线路板上的多个LED芯片; 所述线路板表面覆盖有遮光层;所述反光镜为抛物面反光镜,所述LED光源组件设置在抛物面反光镜的焦点处。 [0011] The object of the present invention is achieved by the following technical solution: a portable liquid food based on digital light processing technology of the near-infrared spectrometer, comprising a LED light source assembly, a mirror, a blazed grating, a digital micromirror assembly, single-photon detector , linear detector and a spectral information processing system, the spectral information processing system is connected to the digital micromirror assembly, single-photon detector, in communication with the linear detector; said LED light source assembly includes a heat-dissipating substrate, a substrate covering the heat and a circuit board mounted on the plurality of LED chips on the circuit board; a circuit board surface is covered with a light shielding layer; the reflector is a parabolic reflector, the LED light source assembly disposed at a focal point of the parabolic reflector.

[0012] 所述光源组件还可以采用下述封装结构,该封装结构包括载体,该载体上设有型腔,该型腔底部设有所述线路板和LED芯片,该型腔内填充有热隔离材料,该型腔表面设有荧光粉层;该荧光粉层包括有机红色荧光粉层与YAG荧光粉层,该有机红色荧光粉层层叠在荧光粉层上。 [0012] The light source assembly may also be employed the following configuration package, the package structure comprises a carrier, on which carrier is provided with a cavity, the bottom of the cavity is provided with an LED chip and the wiring board, the cavity filled with a heat insulating material, the cavity surface provided with the phosphor layer; the phosphor layer comprises a red phosphor layer and an organic layer YAG phosphor, the red phosphor organic layer is stacked on the phosphor layer. 该YAG荧光粉层由YAG荧光粉制成,且该YAG荧光粉为YAG黄色荧光粉或YAG绿色荧光粉。 The YAG phosphor layer is made of a YAG phosphor, the YAG phosphor and a YAG YAG yellow phosphor or green phosphor. 该热隔离材料可以是硅胶或其他同时具有很好热隔离效果和透光率的材料,以保证荧光粉的高量子效率。 The thermally insulating material may be silica gel or other material having good thermal isolation at the same time and the light transmittance, in order to ensure high quantum efficiency of the phosphor. 在本实施例中,均采用硅胶作为热隔离材料。 In the present embodiment, the silica gel are used as a heat insulating material. 有机红色荧光粉层与YAG荧光粉层均为单层,且均为长形薄膜,该有机红色荧光粉层层叠在YAG荧光粉层上形成双层膜结构。 The organic layer and the red phosphor YAG phosphor layer is of single layer, and are elongated film, the organic layer is stacked on the red phosphor YAG phosphor layers form a bilayer membrane structure. 上述技术不但能提高白光LED的高显色指数,同时能保证发光效率低衰减,从而保证良好的发光效率。 Technology not only can improve the above-described white LED high color rendering index, emission efficiency at the same time can guarantee a low attenuation, thus ensuring good emission efficiency. 本技术在于跳出传统白光LED中无机红色荧光粉发光效率低的局限而使用有机红色荧光粉,因有机发光材料具备分子设计灵活、种类繁多、结构和光谱易控、更宽的发光颜色选择、发光效率高、易于大面积成膜、成本低、工艺简单等一系列优势。 This technique consists out of the traditional white LED light emission efficiency of the red phosphor lower inorganic and organic limitations red phosphor, because the organic light emitting material includes a flexible molecular design, a wide range of spectral and easy to control the structure, a wider selection of emission color, the light emitting high efficiency, easy of large area, low cost, simple process and a series of advantages. 这些优势使得有机红色荧光粉在材料本身的制备和改进方面具有很大的优势, 能够为白光LED提供更高的显色指数的同时保证高发光效率。 These advantages make the organic red phosphor has a great advantage in the production and improvement of the material itself can provide higher CRI white LED while ensuring high luminous efficiency. 另外,本技术可以使用于不同的远场封装形式或热隔离封装形式,以保证荧光粉的高量子转换效率同时实现白光LED 的高显色指数及长寿命。 Further, the present technique can be used in different far-field thermal insulation package or packages, to ensure a high color rendering index and long life of the phosphor while achieving high quantum efficiency white LED.

[0013] 进一步的,所述数字微镜器件中的微镜可±12°旋转;所述单光子探测器与微镜+ 12°旋转时的反射光处于同一直线上;所述线性探测器与微镜负12°旋转时的反射光处于同一直线上;所述单光子探测器为单光子雪崩二极管探测器;所述线性探测器为硫化铅光电探测器。 [0013] Further, the digital micromirror devices may be ± 12 ° rotation of the micromirror; a single-photon detector micromirror + 12 ° when reflected light is rotated in the same line; and said linear detector when the micro-mirror reflecting a negative optical rotation of 12 ° on the same line; the single-photon detector is a single photon avalanche diode detector; the linear detector is a lead sulfide photodetector. 所述光谱信息处理系统为德州仪器所产的DLP 4500 NIR芯片组更进一步的,本发明选用DLP 4500 NIR芯片组作为所述光谱信息处理系统,这是一款优化用于近红外光技术的DLP芯片组。 The spectral information processing system produced by Texas Instruments DLP 4500 NIR chipset further, the present invention is selected DLP 4500 NIR chipset as the spectral information processing system, which is an optimization technique for near-infrared light DLP chipset. 可支持快速、可编程模式速率,以及通过使用可靠的本发明的数字微镜器件的反射微电机械系统(MEMS)微镜技术完成数字切换,并对所述线性探测器及单光子探测器的数据进行手机和处理,形成光谱结果。 It can support fast, programmable speed mode, and by using a reflection micro-electro-mechanical systems, reliable digital micromirror device according to the present invention (MEMS) technology to complete the digital micromirror switching, and a linear detector and a single photon detector phone and process data to form spectrum results. 同时,该芯片组可满足本发明所需提供工厂及现场使用的高性能、经济的近红外光谱仪的各式需求。 Meanwhile, the chipset may be required to meet the present invention provides high performance factory and field use, the economic needs of all kinds of near-infrared spectrometer.

[0014] 同时,上述芯片组可借助现有的SDK工具包,将所述数字微镜器件(DMD)技术与摄像机、传感器、汽车或其他外围设备整合,从而轻松实现3D点云的构建。 [0014] Meanwhile, the above chipset by conventional SDK kit, the digital micromirror device (DMD) technology and cameras, sensors, integrated automobile or other peripheral devices to easily build 3D point cloud. SDK的主要优势在于能快速实现可编程模式速率,及使用可靠的反射MEMS微镜技术完成数字切换。 The main advantage is that the SDK Programmable fast speed mode, and the use of reliable MEMS mirror reflection complete digital switching technology.

[0015] 所述LED光源组件还包括设置在LED芯片外侧的聚光透镜;所述聚光透镜包括覆盖在LED芯片外侧的透明圆锥体;所述透明圆锥体侧面包裹有遮光层,遮光层的高度低于圆锥体顶部的高度。 [0015] The LED light source assembly further comprises a condensing lens disposed outside of the LED chip; overlying said condenser lens comprises a transparent LED chips outer cone; the cone side surface wrapped with a transparent light-shielding layer, light shielding layer a height lower than the top of the cone. 所述聚光透镜为高透光聚碳酸酯材料制成,所述高透光聚碳酸酯材料其原料按重量计包括50~70份聚碳酸酯、0. 1~0. 2份阻燃剂、0. 5~0. 9份相容剂以及0. Π 份的石墨烯。 The condenser lens is a polycarbonate material of high transparency, a high transmittance polycarbonate material which comprises a raw material by weight, 50 to 70 parts of a polycarbonate, 0.1 ~ 0.2 parts of a flame retardant , 0.5 ~ 0.9 parts of compatibilizing agent and 0. Π parts graphene. 所述透明圆锥体的高度为抛物面反光镜焦距的0.2~0. 5倍。 Said transparent cone height is 0.2 to 0.5 times the focal length of the parabolic reflector. 高透光的聚碳酸酯,聚碳酸酯其分子结构排列较为整齐,大约是一种层状、线性的排列方式,能够使进入聚碳酸酯材料中的红外光沿一定的方向传递。 High transmittance of the polycarbonate, the polycarbonate is more neatly arranged in its molecular structure, is about a layered, linear arrangement, can be made into the polycarbonate material in the infrared light passing a certain direction. 而石墨烯更是有整齐的单层片状层状结构, 当石墨烯分散在聚碳酸酯中,由于石墨烯间范德华力(van der waals force)的作用,石墨烯将相互平行地分散在聚碳酸酯中,引导红外光沿一定的方向传导。 Graphene is the single-layer sheet-like neatly layered structure, when dispersing the graphene in the polycarbonate, the action of van der Waals force between the graphene (van der waals force), and parallel to one another graphene dispersed in the poly carbonate, guiding the infrared light transmission in a certain direction. 更为优选的,本发明选用磺酰化处理的石墨烯,比如带有甲苯磺酰基的石墨烯(具体见Ping Wen, Peiwei Gong 等人2014年7 月发表于RSC Advances 期刊的"Scalable fabrication of high quality graphene by exfoliation of edge sulfonated graphite for supercapacitor application")。 More preferably, the present invention selects a sulfonyl graphene treatment, such as graphene with tosyl group (particularly see Ping Wen, Peiwei Gong et al., Published in July 2014, RSC Advances journal "Scalable fabrication of high quality graphene by exfoliation of edge sulfonated graphite for supercapacitor application "). 磺酰基为石墨烯分子间提供更强的范德华力,一方面有助于保持聚碳酸酯中石墨烯间平行的层状分布状体,另一方面也有助于提高石墨烯在聚碳酸酯中的分散性, 防止其沉淀。 Sulfonyl between graphene molecules provide stronger van der Waals force, on the one hand between the polycarbonate helps maintain parallel layered graphene-like profile body, on the other hand also help to improve graphene polycarbonate dispersion, prevent its precipitation. 石墨烯会使红外光被遮挡,因此本发明特别限定石墨烯的浓度,在报聚碳酸酯材料透光性的同时最大程度地提高红外光的定向辐射。 Graphene causes infrared light is blocked, and thus the present invention is particularly limited to a concentration of graphene, while packets translucent polycarbonate material increases directional radiation of infrared light maximally. 所述阻燃剂、相容剂均可选用市售的聚碳酸酯用阻燃剂和相容剂实现。 The flame retardant, a compatibilizer can be selected using a commercially available flame retardant polycarbonate and compatibilizing agent implementation. 相容剂主要用于连接聚碳酸酯分子和石墨烯分子,保持石墨烯-聚碳酸酯体系的稳定性。 Compatibilizing agent is used to connect molecules of polycarbonate molecules and graphene, holding graphene - Stability of Polycarbonate. 除此以外,发明人发现添加有石墨烯的聚碳酸酯材料具有优秀的抗老化性能,长期使用仍具有良好的透光度,无裂痕、雾化等瑕疵产生。 In addition, the inventors have found that adding a polycarbonate material graphene has excellent anti-aging properties, long-term use still has a good degree of light transmission, no cracks, and other defects produce atomization.

[0016] 特别优选的,所述透明圆锥体可将LED芯片完全包裹,所述遮光测可以是内侧反光,遮光测则能够防止聚光镜漏光。 [0016] Particularly preferred, said transparent cone LED chip may be completely wrapped, the inside of the light shielding sensing may be reflective, the light blocking condenser lens measuring light leakage can be prevented. LED芯片发出的光线可在聚光镜内部增强,控制当遮光测内侧反光时,控制遮光层的高度还可产生相长干涉。 Light emitted from the LED chip inside the condenser lens can be enhanced, when the light shielding sensing control reflective inside, controlling the height of the light shielding layer may also generate constructive interference. 由于遮光层的高度低于圆锥体顶部, 因此圆锥体顶部未被遮光层包裹,露出部位的俯视投影为一圆形光点。 Since the height of the light-shielding layer below the top cone, the top cone is not so light-shielding layer is wrapped, the exposed portion of the overhead projection of a circular light spot is. 光线最终能从该圆锥体的顶部射出,形成一近似的点光源。 Finally from the top of the light cone emitted, forming an approximate point source.

[0017] 本发明还提供一种采用所述近红外光谱仪快速无损检测果汁中防腐剂的方法。 [0017] The present invention further provides a method for the near-infrared spectrometer juice rapid non-destructive testing of preservative employed.

[0018] 特别优选的,所述防腐剂为苯甲酸类防腐剂,具体包括以下步骤: SI.将样品的温度降温至1 一3°C,加入体积为样品的1% - 5%的浓度为10 - 30mol/mL 的氯化钠水溶液和体积为样品〇. 5%-1%的浓度为3-5mol/mL的石墨烯水悬液,获得粗处理样品; 52. 采用旋转式摇床对粗处理样品进行震荡处理; 53. 将粗处理样品的pH值调节至5. 6 - 6. 1 ; 54. 加热粗处理样品,在30- 40°C下保温静置; 55. 将样品降温至2 - 5°C,对样品进行过滤,收集滤液为初滤液; 56. 将滤渣与体积等于滤液的去离子水混合,并采用真空过滤,收集滤液为洗脱液; 57. 将初滤液与洗脱液混合,采用旋转蒸发仪在30- 40°C下旋转蒸发,直至其体积降至与样品相等,获得结果样品; 58. 采用所述近红外光谱仪测定结果样品中防腐剂的浓度。 [0018] Particularly preferred, the preservative is a benzoate preservatives, comprises the steps of: SI sample temperature was lowered to a 1 3 ° C, was added 1% by volume of the sample - as concentration of 5%. 10 - the volume of aqueous sodium chloride and 30mol / mL for the sample concentration of 5 billion to 1% of 3-5mol / mL graphene aqueous suspension, treating the sample to obtain a crude; 52. the crude rotary shaker. samples were shock treatment process; 53. the pH was adjusted to rough handling of the sample 5.6 - 6.1; 54. thick heat treated sample, at 30- 40 ° C incubation was allowed to stand; the sample was cooled to 55. 2 - 5 ° C, the sample is filtered, the filtrate was collected as the original filtrate; 56. the filter residue with a volume equal to the filtrate was deionized water, and vacuum filtration, the filtrate was collected as the eluent; 57. First the filtrate and eluted mixing liquid, rotary evaporation using a rotary evaporator at 30- 40 ° C, until the volume was reduced and the sample equal to sample results obtained; 58. the use of the near-infrared spectrometer sample measurement result of the concentration of the preservative.

[0019] 所述采用旋转式摇床对粗处理样品进行震荡处理是指以100-300转/min的转速在5-10摄氏度恒温条件下对粗处理样品震荡10- 25min。 [0019] The crude shock treatment for the treated sample using a rotary shaker refers to the speed of 100-300 rpm / min The crude 10- 25min shock treating the sample under constant temperature 5-10 ° C.

[0020] 本发明在采集样品的吸收光谱前,对其进行了一系列的前处理,以提高检测结果的精确度。 [0020] In the present invention, before the absorption spectrum of the sample collection, it was carried out a series of pre-treatment, to improve the accuracy of detection results. 通常而言,果汁中的果胶、蛋白质等不溶的胶体对苯甲酸类的防腐剂有较强的吸附作用,干扰检测并使检测结果远低于实际含量。 In general, in the juice-soluble colloids pectin, proteins, etc. have a strong adsorption of the preservative benzoic acid, and the detection result of the detection of interference is much lower than the actual amount. 设计人发现,在低温及氯化钠、石墨烯存在的条件下,样品中的果胶、蛋白质等大分子悬浮物对该类防腐剂的束缚作用减弱,防腐剂更容易从这些物质中逸散至样品中,采用近红外光谱法测试得的样品防腐剂浓度更为接近其真实数值。 Found design, and sodium chloride at a low temperature, the presence of graphene, the binding effect of the preservatives in the sample pectin, proteins and other macromolecules suspension weakened, preservatives escape more easily from these substances to the sample using near-infrared spectroscopy to obtain a test sample concentration of the preservative is closer to its true value. 所述石墨烯水悬液为市售的石墨烯与水的混合物。 The aqueous suspension is a mixture of graphene and graphene commercially available water. 而震荡处理则能促进大分子悬浮物释放防腐剂的进程。 The shock treatment is able to facilitate the process of release of macromolecules suspended preservative. 在S3的pH条件下对样品进行加热,本来较稳定悬浮在果汁样品中的果汁、蛋白质等物质相互间的范德华力减弱,容易发生絮凝、沉降,有利于后续处理中将其去除。 The samples were heated at a pH S3, had relatively stable suspension in the juice in the juice samples, protein and other substances mutual van der Waals force is weakened, prone to flocculation, settling, will facilitate the subsequent processing thereof is removed. 滤渣的表面通常会吸附有一部分的防腐剂,采用去离子水可将其洗脱并进入滤液中,使检测结果更为精确。 The residue is adsorbed surface is usually a part of preservative, deionized water may be eluted into the filtrate, so that more accurate detection result. 本发明还对滤液与洗脱液的混合物体积进行缩减,使之与样品的原始体积一致,以减少计算检测结果的步骤,提高检测效率的同时还可降低出错率、 提高检测精度。 The present invention is also a mixture of the filtrate and the volume of the eluate is reduced, so identical to the original volume of the sample, in order to reduce the step of calculating the detection result, to improve the detection efficiency while reducing the error rate and improve the detection accuracy. 尤其是对该混合物进行浓缩,还降低对红外光谱仪敏感度的要求,从而压缩检测成本。 The mixture was concentrated in particular, but also reduce the requirements for sensitivity infrared spectrometer, whereby the compression detector costs. 由于苯甲酸类防腐剂耐热性较差,本发明特别选用低温旋蒸的方式对上述混合物进行浓缩,以减少浓缩过程中防腐剂的损失。 Since the preservatives benzoic poor heat resistance, the present invention is especially selected manner and rotary evaporated cryogenic mixture was concentrated, and concentrated in order to reduce losses during preservatives. 步骤8所称采用所述近红外光谱仪测定结果样品中防腐剂的浓度可以本发明的近红外光谱仪为硬件选用任一种测试有机物浓度的方法进行类推适用。 Step 8 NIR spectroscopy mentioned near-infrared spectrometer sample measurement result of the concentration of the preservative can be selected according to the present invention is any hardware organic concentration tested using the analogy applies.

[0021] 进一步的,所述采用红外光谱法测定结果样品中防腐剂的浓度是指采用分析纯的苯甲酸类防腐剂配制不同浓度的果汁标准溶液,获得各浓度的果汁标准溶液的吸收光谱图;使用多元校正方法建立被测样品中防腐剂含量与吸收光谱之间关系的数学模型,并对模型进行验证;获得结果样品的吸收光谱,用所述数学模型计算得结果样品中防腐剂的浓度。 [0021] Further, the measurement results of infrared spectroscopy using sample concentrations of preservative solutions using standard means juice analytically pure acid of different concentrations of formulated preservatives, absorption spectrum of the juice obtained at each concentration of the standard solution ; mathematical model of the relationship between the test sample and the preservative content absorption spectra using multivariate calibration methods, and the model is validated; absorption spectra of samples obtained, the sample calculation results obtained with the mathematical model of the preservative concentration .

[0022] 特别的,本发明所述步骤8参照了申请号为2004101039768的中国发明专利"果汁中阿斯巴甜的近红外光谱快速无损检测方法",并依据苯甲酸类防腐剂的性质对其进行了适应性的修改。 [0022] In particular, the steps of the present invention with reference to the 8 of Chinese Application No. 2004101039768 patent "Detection aspartame sweetened fruit juice Nondestructive Near Infrared Spectroscopy", and according to the nature of its benzoate preservatives were adaptive changes. 其具体操作步骤主要包括: 采用分析纯的防腐剂配制出一系列不同浓度的果汁标准溶液(〇. 1 - 3mg/mL),作为建立数学模型的样品库。 The specific steps include: preservatives formulated using analytically pure juice series of different concentrations of standard solutions -, the establishment of a mathematical model of the sample repository (square 1 3mg / mL.). 将不同防腐剂浓度的果汁标准溶液采用本发明的近红外光谱仪测试,波长范围选定为780nm - 2500。 The juice different preservative concentrations of standard solutions with the present invention the near infrared spectroscopy, the wavelength range selected for the 780nm - 2500. 记录各个标准溶液的吸收光谱。 Recording an absorption spectrum of each standard solution. 使用多元校正方法,具体而言是化学计量学的多元校正方法中的连续波长近红外光谱计算方法和离散波长进红外光谱计算方法建立所述防腐剂含量与吸收光谱之间关系的数学模型。 Using multivariate calibration methods, specifically a continuous wavelength multivariate calibration chemometrics in the near-infrared spectrum into discrete wavelengths calculated and infrared spectrum preservative content calculation method of establishing the mathematical model of the relationship between the absorption spectra. 具体方法可采用所述申请号为2004101039768的中国发明专利中所记载的方法。 The particular method employed is a method of Chinese Patent Application No. 2004101039768 the invention described. 收集结果样品的吸收光谱, 采用上述数学模型便可最终获得样品中防腐剂的浓度(含量)。 Absorption spectrum results of the samples collected, in the mathematical models can be employed to obtain a final concentration (content) of the samples a preservative.

[0023] 所述多元校正方法是化学计量学的多元校正方法。 [0023] The multivariate calibration methods are multivariate chemometric calibration method.

[0024] 本发明相对于现有技术,具有如下的有益效果: 1.本发明提供的近红外光谱分析仪选用多个LED芯片构成的矩阵作为近红外光谱仪中的光源,同时特别在LED芯片外侧设置聚光透镜,进而减小光源的发光面积、保证光源能够提供足够的光强;而LED芯片具有高光强、低功率的特点,有利于减小本发明近红外光谱仪产品的体积,使之更加便携,更加适用于流体食品检测。 [0024] The present invention relative to the prior art, has the following advantages: 1. The near-infrared spectrometer of the present invention provides the selection matrix composed of a plurality of LED chips as the light source in the near-infrared spectrometer, and in particular outside of the LED chip setting a condenser lens, and thus the light emitting area of ​​the light source, to ensure that the light source capable of providing sufficient light intensity; and an LED chip having a high intensity, the characteristics of low power, it is advantageous to reduce the volume of the present invention, near-infrared spectrometer product to make it more portable more suitable for fluid food testing.

[0025] 2.本发明选用DLP 4500 NIR芯片组作为所述光谱信息处理系统,进而提高数据处理效率,缩短数据处理时间,使本发明能够快速、准确地测定流体食品的成分。 [0025] 2. The present invention is selected as a chipset DLP 4500 NIR spectral component of the information processing system, thereby improving data processing efficiency, shorten the data processing time of the present invention can quickly and accurately measure the fluid food.

[0026] 本发明采用红外光谱法检测果汁饮料中的防腐剂浓度,样品前处理简单,无需对防腐剂进行深度提纯,检测效率高于现有的HPLC (液相色谱)法,有利于在大规模的工业化生产中推广。 [0026] The present invention uses infrared spectroscopy detected concentration of fruit juice beverage preservative, simple sample without preservatives depth purification, detection more efficient than a conventional HPLC (liquid chromatography), in favor of large scale industrial production promotion.

[0027] 2.本发明通过对果汁样品进行一系列的简单处理,消除果汁中的果胶、蛋白质等物质对防腐剂检测结果的干扰,其精确度可高至±0. 〇5mg/mL。 [0027] 2. The present invention is by a series of simple juice samples, eliminating the interference in the juice pectin, protein and other substances on the detection result of preservatives, which may be of high accuracy to ± 0. 〇5mg / mL.

附图说明 BRIEF DESCRIPTION

[0028] 图1为本发明的结构示意图。 [0028] FIG. 1 is a schematic structural diagram of the present invention.

[0029] 图2为本发明反光环的局部放大图。 [0029] Fig 2 an enlarged view of the anti-halo present invention.

[0030] 图3是本发明探头本体的原理图。 [0030] FIG. 3 is a schematic diagram of the probe body of the present invention.

[0031] 图4是本发明LED红外光源组件的结构示意图。 [0031] FIG. 4 is a structural diagram of the present invention, an infrared LED light source assembly.

具体实施方式 detailed description

[0032] 为了便于本领域技术人员理解,下面将结合实施例对本发明作进一步详细描述: 实施例1 本实施例提供一种便携的果汁检测红外光谱仪,如图1所示,其包括可手持的外壳1, 设在外壳同一端的光线发射口2及收集反射光线的闪耀光栅3。 [0032] In order to facilitate those skilled in the art understand, the following embodiments in conjunction with the embodiment of the present invention is described in further detail: to provide a portable detector juice infrared spectrometer EXAMPLE 1 This example embodiment shown in Figure 1, which includes a hand-held a housing provided at the same end of the housing 2 and the light emitting port to collect the reflected light blazed grating 3.

[0033] 其内部结构如图2所示,包括LED光源组件21、反光镜、闪耀光栅3、数字微镜组件4、单光子探测器6、线性探测器7以及光谱信息处理系统,所述光谱信息处理系统5与所述数字微镜组件、单光子探测器、线性探测器通信连接;其特征在于:所述LED光源组件包括散热基板、覆盖在散热基板上的柔性线路板以及安装于柔性线路板上的多个LED芯片;所述柔性线路板表面覆盖有反光层;所述反光镜为抛物面反光镜,所述LED光源组件设置在凹面反光镜的焦点处。 [0033] The internal structure shown in Figure 2, comprises a 21, a mirror, a blazed grating 3, a digital micromirror assembly 4, 6 single-photon detector, the detector 7 and the linear spectral information processing system of the LED light source components, the spectral the information processing system connected to said digital micromirror assembly 5, single-photon detector, in communication with the linear detector; characterized in that: the LED light source assembly includes a heat-dissipating substrate, covers the substrate on the heat sink mounted to the flexible wiring board and a flexible circuit a plurality of LED chips board; the flexible circuit board surface is covered with a reflective layer; said reflector is a parabolic reflector, the LED light source assembly disposed at the focal point of the concave mirror. 如图3、图4,所述LED光源组件还包括设置在LED芯片外侧的聚光透镜21 ;所述聚光透,21包括覆盖在LED芯片外侧的透明圆锥体211 ;所述透明圆锥体侧面包裹有遮光层212,遮光层的高度低于圆锥体顶部的高度本实施例还提供一种近红外光谱快速无损检测果汁中防腐剂浓度的方法,包括以下步骤: SI.将样品的温度降温至2°C,加入体积为样品的3%的浓度为25mol/mL的氯化钠水溶液和体积为样品〇. 5%的浓度为3mol/mL的石墨烯水悬液,获得粗处理样品; 52. 采用旋转式摇床对粗处理样品进行震荡处理; 53. 将粗处理样品的pH值调节至6 ; 54. 加热粗处理样品,在30°C下保温静置IOmin; 55. 将样品降温至5°C,对样品进行过滤,收集滤液为初滤液; 56. 将滤渣与体积等于滤液的去离子水混合,并采用在表压为-70KPad的真空过滤,收集滤液为洗脱液; 57. 将初滤液与洗脱液混合,采用旋 3, FIG. 4, the assembly further comprises a LED light source disposed outside the LED chip condenser lens 21; the condensing lens, a transparent cover 21 comprises a conical outer side LED chip 211; the side surface of the transparent cone wrapped with a light-shielding layer 212, the height of the light shielding layer is lower than the height of the top cone according to the present embodiment further provides a near-infrared spectroscopy method of detecting nondestructive preservative fruit juice concentration, comprising the steps of:. SI sample temperature was lowered to . aqueous sodium chloride concentration of 3% by volume of 2 ° C, a volume of sample added was 25mol / mL to a concentration of 5% of the sample was square 3mol / mL graphene aqueous suspension to obtain a crude sample processing; 52. using a rotary shaker for shaking sample handling process crude; crude 53. the pH was adjusted to 6 for processing a sample; 54. thick heat treated sample, incubated at 30 ° C was allowed to stand IOmin; 55. the sample was cooled to 5 ° C, the sample is filtered, the filtrate was collected as the original filtrate; 56. the filter residue with a volume equal to the filtrate was deionized water, and using a gauge pressure of -70KPad vacuum filtration, the filtrate was collected as the eluent; 57. the the filtrate was mixed with the eluate First, spin 蒸发仪在40°C下旋转蒸发,直至其体积降至与样品相等,获得结果样品; 58. 在暗室中将所述光线发射口正对样品,使光线照射样品,采集样品的红外光谱,测定结果样品中防腐剂的浓度。 Rotary evaporator at 40 ° C for evaporation until the volume was reduced and the sample equal to sample results obtained; 58. the light emitted in the darkroom positive sample port, so that the light irradiating the sample, collecting the infrared spectrum of the sample was measured results preservative concentration in the sample.

[0034] 进一步的,所述采用旋转式摇床对粗处理样品进行震荡处理是指以200转/min的转速在5摄氏度恒温条件下对粗处理样品震荡15min。 [0034] Further, using a rotary shaker of the crude sample shock treatment refers to a process speed of 200 revolutions / min. The crude sample was treated 15min shaking at a constant temperature of 5 degrees Celsius.

[0035] 所述采用红外光谱法测定结果样品中防腐剂的浓度是指采用分析纯的苯甲酸钠配制不同浓度的果汁标准溶液,获得各浓度的果汁标准溶液的吸收光谱图;使用多元校正方法建立被测样品中防腐剂含量与吸收光谱之间关系的数学模型,并对模型进行验证;获得结果样品的吸收光谱,用所述数学模型计算得结果样品中防腐剂的浓度。 [0035] The concentration measurement using infrared spectroscopy result of a sample refers to the use of preservatives are sodium benzoate formulated analytically pure standard solutions of different concentrations of the juice, the juice obtained absorption spectrum at each concentration of the standard solution; created using multivariate calibration methods mathematical model of the relationship between the test sample spectra with absorption preservative content, and the model is validated; absorption spectra of samples obtained, the sample calculation results obtained with the mathematical model of the preservative concentration.

[0036] 所述样品为鲜榨葡萄汁与不同浓度的分析纯苯甲酸钠(市售产品)配制而成。 [0036] The sample is analyzed with the freshly squeezed juice of different concentrations of sodium formate benzene (commercial product) preparation. 其检测结果如表1所示。 Detection results shown in Table 1. 平均每个样品(IOmL)的测试时间为30min 对比例1 本对比例提供一种果汁中防腐剂浓度的检测方法,其具体步骤为: 将样品进行过滤,并用去离子水冲洗滤饼,收集滤液。 The average for each sample (IOmL) in a test time of 30min Comparative Example 1 This comparative example provides a method for detecting the concentration of the preservative fruit juice, including the following steps: A sample was filtered and the filter cake was rinsed with deionized water, the filtrate was collected . 对滤液采用旋转蒸发仪在40°C下旋转蒸发,直至其体积降至与样品相等,获得结果样品。 The filtrate was rotary evaporated using a rotary evaporator at 40 ° C, until the volume was reduced and the sample equal to sample the results obtained. 收集该结果样品的吸收光谱,利用实施例1建立的数学模型计算得结果样品的防腐剂浓度,其检测结果如图1所示。 Collecting the results of absorption spectrum of the sample, the concentration of preservative calculated results of the samples in Example 1 by using the mathematical model established detection results shown in Fig. 所述样品为鲜榨葡萄汁与不同浓度的分析纯苯甲酸钠(市售产品)配制而成。 The samples were analyzed fresh juice and various concentrations of sodium formate benzene (commercial product) preparation.

[0037] 对比例2 本对比例提供一种果汁中防腐剂浓度的检测方法,其具体步骤为:将样品的温度降温至2°C,加入体积为样品的3%的浓度为25mol/mL的氯化钠水溶液,获得粗处理样品将样品进行过滤,并用去离子水冲洗滤饼,收集滤液。 [0037] Comparative Example 2 provides a method for detecting the concentration of preservative Comparative fruit juice, including the following steps: The temperature of the sample cooled to 2 ° C, was added to a concentration of 3% by volume of the sample was 25mol / mL of aqueous sodium chloride solution, treating the sample to obtain a crude samples were filtered and the filter cake was rinsed with deionized water, the filtrate was collected. 对滤液采用旋转蒸发仪在40°C下旋转蒸发, 直至其体积降至与样品相等,获得结果样品。 The filtrate was rotary evaporated using a rotary evaporator at 40 ° C, until the volume was reduced and the sample equal to sample the results obtained. 收集该结果样品的吸收光谱,利用实施例1建立的数学模型计算得结果样品的防腐剂浓度,其检测结果如图1所示。 Collecting the results of absorption spectrum of the sample, the concentration of preservative calculated results of the samples in Example 1 by using the mathematical model established detection results shown in Fig. 所述样品为鲜榨葡萄汁与不同浓度的分析纯防腐剂(市售产品)配制而成。 The fresh sample is analytically pure grape juice with different concentrations of the preservative (commercially available product) preparation.

Figure CN105092516AD00081

[0038] 以上为本发明的其中具体实现方式,其描述较为具体和详细,但并不能因此而理解为对本发明专利范围的限制。 Wherein the specific implementation of the [0038] present invention, the above, and detailed description thereof is more specific, but can not therefore be understood as limiting the scope of the present invention. 应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些显而易见的替换形式均属于本发明的保护范围。 It should be noted that those of ordinary skill in the art, without departing from the spirit of the present invention, can make various changes and modifications, obvious alternative forms of these belong to the scope of the present invention.

Claims (15)

  1. 1. 一种基于数字光处理技术的便携式液体食物近红外光谱分析仪,包括LED光源组件、反光镜、聚光透镜、闪耀光栅、数字微镜组件、单光子探测器、线性探测器以及光谱信息处理系统,所述光谱信息处理系统与所述数字微镜组件、单光子探测器、线性探测器通信连接;其特征在于:所述LED光源组件包括散热基板、覆盖在散热基板上的线路板以及安装于线路板上的多个LED芯片;所述柔性线路板表面覆盖有反光层;所述反光镜为抛物面反光镜,所述LED光源组件设置在抛物面反光镜的焦点处;所述LED光源组件还包括设置在LED 芯片外侧的聚光透镜;所述聚光透镜包括覆盖在LED芯片外侧的透明圆锥体;所述透明圆锥体侧面包裹有遮光层,遮光层的高度低于圆锥体顶部的高度。 A portable liquid food based on digital light processing technology of the near-infrared spectrometer, comprising a LED light source assembly, a mirror, a condenser lens, a blazed grating, a digital micromirror assembly, single-photon detector, the detector and the linear spectral information processing system, the spectral information processing system of the digital micromirror assembly, single-photon detector, linear detector communication connection; characterized in that: the LED light source assembly includes a heat-dissipating substrate, covers the substrate on the heat sink and the circuit board circuit board mounted on the plurality of LED chips; the flexible circuit board surface is covered with a reflective layer; said reflector is a parabolic reflector, the LED light source assembly disposed at a focal point of the parabolic reflector; said LED light source assembly further comprising a condenser lens disposed outside of the LED chip; covering said condenser lens comprises a transparent outer cone LED chip; side wrapping said transparent cone with a light shielding layer, the light-shielding layer is lower than the height of the height of the top of the cone .
  2. 2. 根据权利要求1所述的近红外光谱分析仪,其特征在于:所述数字微镜器件中的微镜可±12°旋转;所述单光子探测器与微镜+ 12°旋转时的反射光处于同一直线上;所述线性探测器与微镜负12°旋转时的反射光处于同一直线上;所述单光子探测器为单光子雪崩二极管探测器;所述线性探测器为硫化铅光电探测器;所述光谱信息处理系统为德州仪器所产的DLP 4500 NIR芯片组。 The near-infrared spectroscopic analyzer according to claim 1, wherein: said digital micromirror device of the micromirror may be ± 12 ° rotation; at + 12 ° rotation of the single-photon detector micromirror the reflected light on the same line; reflected when the micromirror of the linear detector with a negative optical rotation of 12 ° on the same line; the single-photon detector is a single photon avalanche diode detector; the linear detector is a lead sulfide a photodetector; the spectral information processing system produced by Texas Instruments DLP 4500 NIR chipset.
  3. 3. -种采用如权利要求1或2所述近红外光谱仪快速无损检测果汁中防腐剂的方法。 3. - species employed to claim 1 or 2 near-infrared spectrometer Nondestructive detection method preservative fruit juice.
  4. 4. 根据权利要求3所述的方法,其特征在于:所述防腐剂为苯甲酸类防腐剂,具体包括以下步骤: 4. The method according to claim 3, wherein: the preservative is benzoic acid-based preservative, comprises the steps of:
  5. 51. 将样品的温度降温至1一3°C,加入体积为样品的1%-5%的浓度为10-30mol/mL 的氯化钠水溶液和体积为样品〇. 5%-1%的浓度为3-5mol/mL的石墨烯水悬液,获得粗处理样品; Aqueous sodium chloride and 1% to 5% by volume concentration of 51. The temperature of the sample is lowered to a 1 3 ° C, a volume of sample was added 10-30mol / mL for the sample square. A concentration of 5% to 1% an aqueous suspension of graphene 3-5mol / mL to obtain a crude sample processing;
  6. 52. 采用旋转式摇床对粗处理样品进行震荡处理; Using a rotary shaker 52. The crude sample shock treatment process;
  7. 53. 将粗处理样品的pH值调节至5. 6 - 6. 1 ; 53. The treated crude sample pH adjusted to 5.6 - 6.1;
  8. 54. 加热粗处理样品,在30-40°C下保温静置; 54. The heat treated crude samples were incubated at 30-40 ° C was allowed to stand;
  9. 55. 将样品降温至2 - 5°C,对样品进行过滤,收集滤液为初滤液; 55. The sample was cooled to 2 - 5 ° C, the sample is filtered, the filtrate was collected as primary filtrate;
  10. 56. 将滤渣与体积等于滤液的去离子水混合,并采用真空过滤,收集滤液为洗脱液; 56. The filter residue with equal volume of the filtrate was mixed with deionized water, and vacuum filtration, the filtrate was collected as the eluent;
  11. 57. 将初滤液与洗脱液混合,采用旋转蒸发仪在30- 40°C下旋转蒸发,直至其体积降至与样品相等,获得结果样品; 57. The beginning of the filtrate was mixed with the eluate, rotary evaporation using a rotary evaporator at 30- 40 ° C, until the volume was reduced to equal the sample, the sample results obtained;
  12. 58. 采用所述近红外光谱仪测定结果样品中防腐剂的浓度。 58. The near-infrared spectrometer using a sample concentration of preservative in the measurement result.
  13. 5. 根据权利要求4的方法,其特征在于:所述采用旋转式摇床对粗处理样品进行震荡处理是指以100- 300转/min的转速在5 -10摄氏度恒温条件下对粗处理样品震荡10- 25min〇 The method according to claim 4, wherein: said rotary shaker crude sample shock treatment process refers to the speed 100-300 rpm / min The crude sample treated at a constant temperature of 5-10 degrees Celsius shock 10- 25min〇
  14. 6. 根据权利要求5所述的方法,其特征在于:所述测定结果样品中防腐剂的浓度是指采用分析纯的防腐剂配制不同浓度的果汁标准溶液,获得各浓度的果汁标准溶液的吸收光谱图;使用多元校正方法建立被测样品中防腐剂含量与吸收光谱之间关系的数学模型,并对模型进行验证;获得结果样品的吸收光谱,用所述数学模型计算得结果样品中防腐剂的浓度。 6. The method as claimed in claim 5, wherein: the measurement results of the samples in preservative concentration refers to fruit juice using standard analytical grade preservative solutions formulated at different concentrations, the concentration of fruit juice to obtain the absorption of each standard solution spectra; multivariate calibration method using a mathematical model of the relationship between the test sample and the absorption spectrum preservative content, and the model is validated; absorption spectra of samples obtained, calculated using the mathematical model results obtained sample preservative concentration.
  15. 7. 根据权利要求6所述的方法,其特征在于:所述多元校正方法是化学计量学的多元校正方法。 7. The method according to claim 6, wherein: said multivariate calibration methods are multivariate chemometric calibration method.
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