Quantitative detection

定量检测
  • 文章类型: Journal Article
    新辉陈皮(XHCP)是一种众所周知的陈皮(CP),广泛用作中草药和食品成分。虽然以前的研究已经探讨了CP的质量如何随时间变化,专门针对XHCP的研究有限。本研究旨在根据总黄酮含量(TF)评估XHCP的化学成分和质量,抗氧化活性(AA),和颜色值(CV)在两个阶段:新鲜收获(XHCP-0Y)和储存3年后(XHCP-3Y)。确定了38种常见的挥发性化合物,以及其中17种化合物的含量,九种非挥发性化合物,其中包括一种生物碱(辛弗林),三种酚酸(PA,原儿茶酸,香草酸,和阿魏酸),和五种类黄酮(纳鲁鲁丁,橙皮苷,sinensetin,景天苷,和橘皮素),首先采用新开发的气相色谱-质谱(GC-MS)和超高效液相色谱(UPLC)方法进行检测。与XHCP-0Y相比,XHCP-3Y中17种挥发性化合物和辛弗林的含量有不同程度的下降,而PA的含量,五种类黄酮,TF,AA,CV增加。挥发性化合物引起的干燥减少和与PA相关的功效增强,黄酮类化合物,和AA建议XHCP在储存3年后质量得到改善。本研究中开发的方法显示了在老化过程中评估XHCP质量的前景。
    Xinhui Chenpi (XHCP) is a well-known type of Chenpi (CP) widely used as both a Chinese herb and a food ingredient. While previous studies have explored how the quality of CP changes over time, there has been limited research specifically on XHCP. This study aims to assess the chemical components and quality of XHCP based on total flavonoid content (TF), antioxidant activity (AA), and color value (CV) at two stages: freshly harvested (XHCP-0Y) and after 3 years of storage (XHCP-3Y). Thirty-eight common volatile compounds were identified, and the content of 17 compounds among them, nine nonvolatile compounds, which included one alkaloid (synephrine), three phenolic acids (PA, protocatechuic acid, vanillic acid, and ferulic acid), and five flavonoids (narirutin, hesperidin, sinensetin, nobiletin, and tangeretin), were firstly detected by the newly developed gas chromatograph-mass spectrometer (GC-MS) and ultra-performance liquid chromatography (UPLC) methods. Compared to XHCP-0Y, the content of 17 volatile compounds and synephrine decreased in XHCP-3Y to varying degrees, while the content of PA, five flavonoids, TF, AA, and CV increased. The reduction of dryness caused by volatile compounds and the enhancement of efficacy related to PA, flavonoids, and AA suggested improved quality of XHCP after 3 years of storage. The methods developed in this study show promise for evaluating the quality of XHCP during the aging process.
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  • 文章类型: Journal Article
    实时,食品风味化合物的精确定性和定量传感对于确保食品安全至关重要,质量,和消费者的接受度。作为食品风味标签的指标,深入研究食品风味化合物的具体成分和含量,以评估食品风味质量至关重要,但仍然面临着巨大的挑战。光致发光荧光探针技术,具有快速检测和高灵敏度,在检测食品风味化合物方面显示出巨大的潜力。在这次审查中,详细介绍了光致发光荧光探针技术的分类和光学传感机理。此外,概述了应用光致发光荧光探针技术分析食品风味化合物所面临的挑战,并指出了未来的研究方向。希望本文能为光致发光荧光探针技术在食品风味质量评价中的应用提供参考。
    The real-time, precise qualitative and quantitative sensing of food flavor compounds is crucial for ensuring food safety, quality, and consumer acceptance. As indicators for food flavor labeling, it is vital to delve deep into the specific ingredient and content of food flavor compounds to assess the food flavor quality, but still facing huge challenges. Photoluminescent fluorescent probe technology, with fast detection and high sensitivity, has shown immense potentials in detecting food flavor compounds. In this review, the classification and optical sensing mechanism of photoluminescent fluorescent probe technology are described in detail. Besides, challenges in applying photoluminescent fluorescent probe technology to analyze food flavor compounds are outlined to indicate future research directions. We hope this review can provide an insight for the applications of photoluminescent fluorescent probe technology in the evaluation of food flavor quality in future.
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  • 文章类型: Journal Article
    背景:在环境监测和核应急领域,为了获得铀酰引起的环境污染和核事故的相关信息,有必要建立一种快速定量的铀酰离子分析技术。作为一种新的有前途的技术,表面增强拉曼散射(SERS)有望实现这一目标。然而,在酸性条件下,铀酰离子很容易从SERS底物中解吸,强酸性水溶液中SERS基底的结构将被破坏。此外,SERS对铀酰离子的定量检测能力有待提高。因此,有必要开发新的SERS基底,以准确定量检测环境水样中的痕量uranyl,尤其是在酸性溶液中。
    结果:在这项工作中,制备了银离子/海藻酸钠超分子水凝胶膜(Ag+/SASMH膜),在激光照射下,膜中的Ag离子转化为Ag/Ag2O复合纳米颗粒。在Ag纳米颗粒的电磁增强与铀酰和Ag2O之间的电荷转移增强的协同作用下,铀酰的拉曼信号强烈增强。利用SA的峰(550cm-1)作为内标,由于铀酰浓度从1.0×10-8molL-1到2×10-6molL-1具有良好的线性关系,因此可以实现LOD为6.7×10-9molL-1的定量检测。此外,外来金属离子几乎不影响铀的SERS检测,该底物可以测定天然水样中的痕量铀酰。特别是,酸度对铀酰离子的SERS信号无明显影响。因此,除了检测天然水样中的铀酰离子,所提出的策略还可以检测强酸性溶液中的铀酰离子。
    首次使用简单的一步法制备了用于快速定量检测铀酰离子的Ag/SASMH膜。所提出的底物通过将铀酰离子固定在水凝胶结构中,在酸性条件下成功检测到铀酰离子。与以前的研究相比,通过使用内标实现了对铀酰离子的更准确的定量分析,所提出的策略可以确定天然水样品或强酸性溶液中的痕量铀酰。
    BACKGROUND: In the fields of environmental monitoring and nuclear emergency, in order to obtain the relevant information of uranyl-induced environmental pollution and nuclear accident, it is necessary to establish a rapid quantitative analytical technique for uranyl ions. As a new promising technique, surface-enhanced Raman scattering (SERS) is hopeful to achieve this goal. However, uranyl ions are easily desorbed from SERS substrates under acidic conditions, and the structures of SERS substrates will be destroyed in the strong acidic aqueous solutions. Besides, the quantitative detection ability of SERS for uranyl ions needs to be promoted. Hence, it is necessary to develop new SERS substrates for accurate quantitative detection of trace uranyl in environmental water samples, especially in acidic solutions.
    RESULTS: In this work, we prepared silver ions/sodium alginate supramolecular hydrogel membrane (Ag+/SA SMH membrane), and the Ag+ ions from the membrane were transformed into Ag/Ag2O complex nanoparticles under laser irradiation. The Raman signal of uranyl was strongly enhanced under the synergistic interaction of electromagnetic enhancement derived from the Ag nanoparticles and charge transfer enhancement between uranyl and Ag2O. Utilizing the peak of SA (550 cm-1) as an internal standard, a quantitative detection with a LOD of 6.7 × 10-9 mol L-1 was achieved due to a good linear relation of uranyl concentrations from 1.0 × 10-8 mol L-1 to 2 × 10-6 mol L-1. Furthermore, foreign metal ions hardly affected the SERS detection of uranyl, and the substrate could determine trace uranyl in natural water samples. Particularly, the acidity had no obvious effect on SERS signals of uranyl ions. Therefore, in addition to the detection of uranyl ions in natural water samples, the proposed strategy could also detect uranyl ions in strong acidic solutions.
    UNASSIGNED: A simple one-step method was used to prepare an Ag+/SA SMH membrane for rapid quantitative detection of uranyl ions for the first time. The proposed substrate successfully detected uranyl ions under acidic conditions by immobilizing uranyl ion in hydrogel structure. In comparison with the previous studies, a more accurate quantitative analysis for uranyl ions was achieved by using an internal standard, and the proposed strategy could determine trace uranyl in either natural water samples or strong acidic solutions.
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  • 文章类型: Journal Article
    轨道不平顺直接影响铁道车辆的运行质量和安全。轨道不规则的定量检测和实时监测具有重要意义。然而,由于车辆速度频繁变化,车辆运行是一个典型的非平稳过程。传统的信号分析方法不适合非平稳过程,使得轨道不规则的波长和振幅的定量检测变得困难。为了解决上述问题,本文首次提出了一种通过阶次跟踪分析来定量检测非平稳条件下车辆行驶不平顺的方法。首先,建立了简化的轮轨动力学模型,推导了车轴箱竖向振动与轨道竖向不平顺之间的定量关系。其次,提出了基于车轴箱垂直加速度的Simpson二重积分方法来计算车轴箱垂直位移,并优化了工艺误差。第三,基于订单跟踪分析理论,结合车轮转速信号对车轴箱垂直位移时域信号进行角域重采样,实现了轨道不规则性的定量检测。最后,基于仿真和现场测试分析案例对所提方法进行了验证。为轨道不平顺的定量检测方法提供理论支持和方法参考。
    Track irregularities directly affect the quality and safety of railway vehicle operations. Quantitative detection and real-time monitoring of track irregularities are of great importance. However, due to the frequent variable vehicle speed, vehicle operation is a typical non-stationary process. The traditional signal analysis methods are unsuitable for non-stationary processes, making the quantitative detection of the wavelength and amplitude of track irregularities difficult. To solve the above problems, this paper proposes a quantitative detection method of track irregularities under non-stationary conditions with variable vehicle speed by order tracking analysis for the first time. Firstly, a simplified wheel-rail dynamic model is established to derive the quantitative relationship between the axle-box vertical vibration and the track vertical irregularities. Secondly, the Simpson double integration method is proposed to calculate the axle-box vertical displacement based on the axle-box vertical acceleration, and the process error is optimized. Thirdly, based on the order tracking analysis theory, the angular domain resampling is performed on the axle-box vertical displacement time-domain signal in combination with the wheel rotation speed signals, and the quantitative detection of the track irregularities is achieved. Finally, the proposed method is validated based on simulation and field test analysis cases. We provide theoretical support and method reference for the quantitative detection method of track irregularities.
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  • 文章类型: Journal Article
    柔性和透明的表面增强拉曼散射(SERS)基底因其能够直接原位检测弯曲表面上的分析物的能力而引起了极大的关注。然而,在测量过程中,物体的曲率会影响SERS的信号增强。在这里,我们提出了一种简单的方法,通过将银纳米颗粒(AgNP)沉积到大面积起皱的聚苯乙烯/聚二甲基硅氧烷(AgNP@W-PS/PDMS)双层薄膜上来制造曲率不敏感的透明SERS基底。使用罗丹明6G(R6G)作为探针分子,优化的AgNP@W-PS/PDMS薄膜显示出4.83×105的高分析增强因子(AEF),优异的均匀性(RSD=7.85%)和重现性(RSD=3.09%),以及优越的机械灵活性。此外,在不同曲率的物体上原位测量孔雀石绿(MG),包括鱼,苹果,还有蓝莓,使用便携式拉曼系统进行,揭示了一致的SERS增强。此外,拉曼强度与从这些物体中检测到的MG的对数浓度之间具有稳健的线性关系(R2≥0.990)。这些结果证明了开发的曲率不敏感SERS基板作为即时测试(POCT)平台用于识别不规则物体上的分析物的巨大潜力。
    Flexible and transparent surface-enhanced Raman scattering (SERS) substrates have attracted considerable attention for their ability to enable the direct in situ detection of analytes on curved surfaces. However, the curvature of an object can impact the signal enhancement of SERS during the measurement process. Herein, we propose a simple approach for fabricating a curvature-insensitive transparent SERS substrate by depositing silver nanoparticles (Ag NPs) onto a large-area wrinkled polystyrene/polydimethylsiloxane (Ag NP@W-PS/PDMS) bilayer film. Using rhodamine 6G (R6G) as a probe molecule, the optimized Ag NP@W-PS/PDMS film demonstrates a high analytical enhancement factor (AEF) of 4.83 × 105, excellent uniformity (RSD = 7.85%) and reproducibility (RSD = 3.09%), as well as superior mechanical flexibility. Additionally, in situ measurements of malachite green (MG) on objects with diverse curvatures, including fish, apple, and blueberry, are conducted using a portable Raman system, revealing a consistent SERS enhancement. Furthermore, a robust linear relationship (R2 ≥ 0.990) between Raman intensity and the logarithmic concentration of MG detected from these objects is achieved. These results demonstrate the tremendous potential of the developed curvature-insensitive SERS substrate as a point-of-care testing (POCT) platform for identifying analytes on irregular objects.
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  • 文章类型: Journal Article
    先前的大多数研究认为,植物真菌病通过空气传播的真菌孢子广泛而迅速地传播。然而,对释放动力学知之甚少,空气动力学直径,温室环境空气中真菌孢子的致病性阈值。葡萄灰霉病是由灰葡萄孢菌引起的;这种疾病通过空气中的孢子在温室中传播,孢子附着在叶子上并通过孔口感染植物。在这项研究中,120μmol/L单叠氮化丙啶(PMA)适用于实时定量PCR处理和定量活孢子,孢子悬浮液中的极限检测为8个孢子/mL。总的来说,通过便携式采样器从葡萄温室的空气样品中分离并鉴定了93株具有高致病性的灰霉病菌。灰霉病菌气溶胶的粒径主要在0.65-3.3μm之间,占总金额的71.77%。灰白芽孢杆菌孢子气溶胶对健康的葡萄植物有感染,可能导致疾病的最低浓度为42孢子/m3。通过PMA-qPCR对山东省六个温室中收集的灰葡萄孢菌孢子进行定量,5月和6月浓度较高(1182.89孢子/m3),7月和8月浓度较低(6.30孢子/m3)。这项研究表明,气溶胶中的孢子传播是植物真菌病流行病学的重要途径。这些数据将有助于制定有效缓解和控制植物病害的新策略。
    Most previously studies had considered that plant fungal disease spread widely and quickly by airborne fungi spore. However, little is known about the release dynamics, aerodynamic diameter, and pathogenicity threshold of fungi spore in air of the greenhouse environment. Grape gray mold is caused by Botrytis cinerea; the disease spreads in greenhouses by spores in the air and the spore attaches to the leaf and infects plant through the orifice. In this study, 120 μmol/L propidium monoazide (PMA) were suitable for treatment and quantitation viable spore by quantitative real-time PCR, with a limit detection of 8 spores/mL in spore suspension. In total, 93 strains of B. cinerea with high pathogenicity were isolated and identified from the air samples of grapevines greenhouses by a portable sampler. The particle size of B. cinerea aerosol ranged predominately from 0.65-3.3 μm, accounting for 71.77% of the total amount. The B. cinerea spore aerosols were infective to healthy grape plants, with the lowest concentration that could cause disease being 42 spores/m3. Botrytis cinerea spores collected form six greenhouse in Shandong Province were quantified by PMA-qPCR, with a higher concentration (1182.89 spores/m3) in May and June and a lower concentration in July and August (6.30 spores/m3). This study suggested that spore dispersal in aerosol is an important route for the epidemiology of plant fungal disease, and these data will contribute to the development of new strategies for the effective alleviation and control of plant diseases.
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  • 文章类型: Journal Article
    长链非编码RNA(lncRNA)作为转录调节因子在疾病中具有重要作用,mRNA加工调节剂和蛋白质合成因子。然而,传统的检测lncRNA的方法耗时耗力,lncRNA的功能仍在探索中。这里,我们提出了一种基于表面增强拉曼光谱(SERS)的生物传感器,用于检测与肝癌(LC)相关的lncRNA以及原位细胞成像。使用双SERS探头,lncRNA(DAPK1-215)的定量检测可以通过靶触发的核心卫星纳米结构的组装以952aM的超低检测限实现。并且该测定的可靠性可以通过能够进行信号动态校准的内标探针以0.9923的R2值进一步提高。同时,使用SERS成像方法,与正常细胞相比,在LC细胞中观察到DAPK1-215主要分布在细胞质中的高表达。此外,细胞功能检测结果显示,DAPK1-215通过显著降低死亡相关蛋白激酶结构域的表达,促进LC的迁移和侵袭。这种基于SERS的生物传感器的开发可以为探索lncRNA的表达提供灵敏而特异的方法,lncRNA将是筛选LC的潜在生物标志物。
    Long-stranded non-coding RNAs (lncRNA) have important roles in disease as transcriptional regulators, mRNA processing regulators and protein synthesis factors. However, traditional methods for detecting lncRNA are time-consuming and labor-intensive, and the functions of lncRNA are still being explored. Here, we present a surface enhanced Raman spectroscopy (SERS) based biosensor for the detection of lncRNA associated with liver cancer (LC) as well as in situ cellular imaging. Using the dual SERS probes, quantitative detection of lncRNA (DAPK1-215) can be achieved with an ultra-low detection limit of 952 aM by the target-triggered assembly of core-satellite nanostructures. And the reliability of this assay can be further improved with the R2 value of 0.9923 by an internal standard probe that enables the signal dynamic calibration. Meanwhile, the high expression of DAPK1-215 mainly distributed in the cytoplasm was observed in LC cells compared with the normal ones using the SERS imaging method. Moreover, results of cellular function assays showed that DAPK1-215 promoted the migration and invasion of LC by significantly reducing the expression of the structural domain of death associated protein kinase. The development of this biosensor based on SERS can provide a sensitive and specific method for exploring the expression of lncRNA that would be a potential biomarker for the screening of LC.
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  • 文章类型: Journal Article
    铀是民用和军事领域的重要核材料;然而,它的广泛应用引起了人们对环境保护和核工业领域潜在安全问题的关注。在这项研究中,我们开发了Ag/Ag2O-COF(共价有机框架)复合SERS基底,以检测环境水溶液中的铀酰离子(UO22)。在这里,将Ag/Ag2O复合材料吸附铀酰的强SERS效应和COFTpPa-1的高吸附效率相结合,实现了对铀酰离子的痕量检测。该方法显示,铀酰离子的线性范围为10-8molL-1至10-6molL-1,检出限为8.9×10-10molL-1。此外,常见的金属阳离子和氧代离子几乎不影响铀的SERS检测,有助于天然水样中铀酰的痕量分析。尽管拟议的策略已用于铀酰检测,可重复使用的高效系统可以扩展到具有拉曼活性的其他物质的痕量检测。
    Uranium is an essential nuclear material in civilian and military areas; however, its extensive application raises concerns about the potential safety issues in the fields of environmental protection and nuclear industry. In this study, we developed an Ag/Ag2O-COF (covalent-organic framework) composite SERS substrate to detect uranyl ions (UO22+) in environmental aqueous solutions. Herein, the strong SERS effect of uranyl adsorbed in Ag/Ag2O composite and the high adsorption efficiency of COF TpPa-1 were combined to realize the trace detection of uranyl ions. This method displayed a linear range of 10-8 mol L-1 to 10-6 mol L-1 with the detection limit of 8.9 × 10-10 mol L-1 for uranyl ions. Furthermore, common metal cations and oxo-ions hardly affected the SERS detection of uranyl, which is helpful for the trace analysis of uranyl in natural water samples. Although the proposed strategy is deployed for uranyl detection, the reusable and high-efficiency system may be expanded to trace detection of other substance with Raman activity.
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  • 文章类型: Journal Article
    为了设计具有多重传感功能的有机小分子荧光材料,合成了双分支化的-NH2修饰的氰基二苯乙烯衍生物(AM)。它表现出溶剂和聚集诱导的发射效应,固态量子产率为28%,比THF高七倍。合成的样品AM通过荧光“关闭”响应对痕量水表现出高灵敏度,在THF中达到0.41µM的低检测限,在EtOH中达到0.80µM。AM还对苦味酸表现出“关闭”反应,归因于它诱导的光诱导电子转移效应。AM对苦味酸的识别显示了对硝基炸药干扰的特异性和抗性,检出限为300ppb,在0-4当量AM范围内呈线性关系(R2=0.9981)。这种酸识别可以促进定性测试纸和安全油墨的设计。此外,AM可以用作在25-110°C的温度范围内具有线性关系(R2=0.9976)的温度传感器。利用这些独特的特征,提出了一系列直接定量测定非水溶剂中痕量水的方法,苦味酸,和温度。
    In order to design organic small molecule fluorescent materials with multiple sensing, a bibranched -NH2 modified cyanostilbene derivative (AM) was synthesized. It exhibits solvent and aggregation-induced emission effects, with a solid-state quantum yield of 28%, which is seven times higher than that in THF. The synthesized sample AM demonstrated high sensitivity to trace water via a fluorescence \"turn-off\" response, achieving a low detection limit of 0.41 µM in THF and 0.80 µM in EtOH. AM also exhibits a \"turn-off\" response to picric acid, attributed to the photo-induced electron transfer effect it induces. The recognition of picric acid by AM demonstrates specificity and resistance to interference from nitro explosives, with a detection limit of 300 ppb and a linear relationship (R2 = 0.9981) at the range of 0-4 equivalents AM. Such acid recognition can facilitate the design of qualitative test papers and safety inks. Additionally, AM can function as a temperature sensor with a linear relationship (R2 = 0.9976) within the temperature range of 25-110 °C. Leveraging these unique characteristics, a series of methods were proposed for the direct quantitative determination of trace water in nonaqueous solvents, picric acid, and temperature.
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  • 文章类型: Journal Article
    抗生素菌丝体残留物(AMR)含有抗生素残留物。如果牲畜过量摄入AMR,它可能会导致健康问题。为了解决当前NIR-HSI中像素尺度掺杂浓度未知的问题,本文创新性地提出了一种新的光谱模拟方法,用于蛋白质饲料中AMR的评价。四种常见的蛋白饲料(豆粕(SM),含可溶物的干酒糟(DDGS),棉籽粕(CM),选择核苷酸残基(NR)和土霉素残基(OR)作为研究材料。该方法的第一步是使用线性混合模型(LMM)模拟具有不同掺杂浓度的像素的光谱。然后,基于模拟像素谱结合基于全局PLS评分的局部PLS(LPLS-S)建立了像素尺度OR定量模型(该模型解决了由于校正集的0%-100%含量而导致的预测结果的非线性分布问题).最后,该模型用于定量预测高光谱图像中每个像素的OR含量。计算每个像素的平均值作为该样品的OR含量。该方法的实施可以有效克服PLS-DA无法实现对2%-20%掺假样品中OR的定性鉴定的问题。与通过平均感兴趣区域的光谱建立的PLS模型相比,这种方法利用每个像素的精确信息,从而提高掺假样品检测的准确性。结果表明,模拟光谱法和LPLS-S的结合为NIR-HSI检测和分析非法饲料添加剂提供了一种新的方法。
    Antibiotic mycelia residues (AMRs) contain antibiotic residues. If AMRs are ingested in excess by livestock, it may cause health problems. To address the current problem of unknown pixel-scale adulteration concentration in NIR-HSI, this paper innovatively proposes a new spectral simulation method for the evaluation of AMRs in protein feeds. Four common protein feeds (soybean meal (SM), distillers dried grains with solubles (DDGS), cottonseed meal (CM), and nucleotide residue (NR)) and oxytetracycline residue (OR) were selected as study materials. The first step of the method is to simulate the spectra of pixels with different adulteration concentrations using a linear mixing model (LMM). Then, a pixel-scale OR quantitative model was developed based on the simulated pixel spectra combined with local PLS based on global PLS scores (LPLS-S) (which solves the problem of nonlinear distribution of the prediction results due to the 0%-100% content of the correction set). Finally, the model was used to quantitatively predict the OR content of each pixel in hyperspectral image. The average value of each pixel was calculated as the OR content of that sample. The implementation of this method can effectively overcome the inability of PLS-DA to achieve qualitative identification of OR in 2%-20% adulterated samples. In compared to the PLS model built by averaging the spectra over the region of interest, this method utilizes the precise information of each pixel, thereby enhancing the accuracy of the detection of adulterated samples. The results demonstrate that the combination of the method of simulated spectroscopy and LPLS-S provides a novel method for the detection and analysis of illegal feed additives by NIR-HSI.
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