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1.
三维荧光光谱结合二阶校正方法测定细胞培养基中阿霉素的含量 总被引:1,自引:0,他引:1
本文采用交替三线性分解(ATLD)和交替归一加权残差三线性分解(ANWE)两种二阶校正方法结合激发发射矩阵荧光光谱对完全不经任何预处理的细胞培养基中的阿霉素进行简单、快速、直接的定量测定.当算法选取组分数为2时,解析得到细胞培养基中阿霉素的平均回收率分别为(100.5±1.8)%和(100.3±1.9)%.在细胞培养基中加入烟酰胺腺嘌呤二核苷酸(NADH)、烟酰胺腺嘌呤二核苷酸磷酸(NADPH)、黄素腺嘌呤二核苷酸(FAD)和黄素单核苷酸(FMN)四种细胞内的自发荧光物后,选取组分数为4时,解析得到细胞培养基中阿霉素的平均回收率分别为(99.1±2.9)%和(99.2±3.1)%.结果表明该分析方法能够准确、快速地直接测定细胞培养基中阿霉素的含量,并且在模拟细胞内荧光干扰环境下可定量测定阿霉素,且能获得令人满意的结果. 相似文献
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将三维荧光光谱技术与秩消失因子分析、广义秩消失因子分析和交替三线性分解3种二阶校正方法相结合,建立了测定未知混合物中苯酚含量的三维荧光二阶校正新方法。设定在激发波长240~280 nm和发射波长280~360 nm范围内测定未知混合物中苯酚的三维荧光光谱,构建三维响应数据阵,运用基于三线性分解的二阶校正算法进行解析。结果表明,当模拟样品的组分数为2时,秩消失因子分析、广义秩消失因子分析和交替三线性分解3种方法测定苯酚的预测均方根误差分别为0.33,1.18和0.15,平均回收率分别为101.6%,115.6%和101.9%;当组分数为3时,3种方法的预测均方根误差则分别为1.61,1.80和0.51,平均回收率分别为134.2%,133.9%和107.1%;将其分别应用于实际样品中苯酚的测定,结果满意,且交替三线性分解法的测定结果优于秩消失因子分析法和广义秩消失因子分析法。 相似文献
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Qingjuan Han Hailong Wu Jinfang Nie Alin Xia Shaohua Zhu Ruqin Yu 《Frontiers of Chemistry in China》2008,3(2):224-228
The concentration of reserpine in urine was directly and quantitatively measured by using the excitation-emission fluorescence
(EEM) combined with three-way calibration methodologies. Two calibration methods are based on the alternating trilinear decomposition
(ATLD) and the self-weighted alternating trilinear decomposition (SWATLD) algorithms, respectively. These chemometric methodologies
have the second-order advantage, which is the ability to get accurate concentration estimates of interested analyte(s) even
in the presence of uncalibrated interferences. The satisfactory results on spiked urine samples are obtained, when the component
number was chosen to 3 (N = 3) for both the methods. This experiment is easily carried out without time-consuming and complicated pretreatment. It
has proved that the three-way calibration methodologies based on ATLD and SWATLD can be feasible to directly quantify the
medical content of reserpine in urine.
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Translated from Chemical Journal of Chinese Universities, 2007, 28 (5): 827–830 [译自: 高等学校化学学报] 相似文献
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本文利用化学计量学交替拟合残差(AFR)算法与高效液相色谱-二极管阵列检测(HPLC-DAD)方法相结合,同时测定两种抗结核药物异烟肼和吡嗪酰胺的含量。该法与交替三线性分解算法(ATLD)、自加权交替三线性分解(SWATLD)算法相比较,从预测均方差、预测相对误差以及平均回收率等结果来看,其预测结果更接近实际值。研究表明,基于交替拟合残差等算法的二阶校正法,可以迅速准确地给出色谱重叠情况下两个组分的预测结果,是复杂体系成分直接定量分析的一个有力的化学计量学工具。 相似文献
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利用三维荧光光谱与化学计量学二阶校正算法相结合, 直接测定人体血浆中和厚朴药材中的厚朴酚及和厚朴酚. 采用平行因子分析(PARAFAC)算法解析所得两种物质的回收率分别为(99.5±2.6)%和(90.2±1.8)%. 采用交替三线性分解(ATLD)算法解析, 当组分数N取3时, 回收率分别为(104.2±3.2)%和(98.7±4.0)%; 当N取4时, 回收率分别为(102.7±2.9)%和(99.0±4.6)%. 同时用该方法对厚朴药材中的厚朴酚及和厚朴酚进行快速定量测定, 结果令人满意. 实验结果表明, 此法可用于复杂试样中未知干扰共存下厚朴酚及和厚朴酚的同时测定. 相似文献
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交替三线性分解算法与反相高效液相-二极管阵列检测方法相结合同时测定苯二酚的位置异构体 总被引:3,自引:0,他引:3
利用交替三线性分解算法与反相高效液相 二极管阵列检测 (RP HPLC DAD)相结合 ,在洗脱时间为1 0 86min~ 1 399min(间隔 1 / 1 50min)、紫外吸收波长为 2 68nm~ 2 98nm(间隔 1nm)时对苯二酚位置异构体的重叠及光谱体系进行了分辨研究。分辨结果与实际结果一致。同时测定了水溶液中共存的邻苯二酚、间苯二酚和对苯二酚的含量 ,回收率分别为 (1 0 0 1± 1 0 ) % ,(99 4± 1 4) % ,(1 0 0 5± 1 7) %。研究结果表明 :该方法定量快速准确 ,实验操作步骤简单 ,解决了在干扰物存在条件下三者很难同时分辨的问题。 相似文献
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Zhang Y Wu HL Xia AL Zhu SH Han QJ Yu RQ 《Analytical and bioanalytical chemistry》2006,386(6):1741-1748
In this study a new spectrofluorimetric method for the direct determination of metoprolol in human plasma is presented and
discussed. It is based on the use of fluorescence excitation–emission matrices (EEMs) and second-order calibration performed
with parallel factor analysis (PARAFAC) or alternating trilinear decomposition (ATLD). This methodology enables accurate and
reliable discrimination of the analyte signal, even in the presence of unknown and uncalibrated fluorescent component(s),
which is often referred to as the second-order advantage. No separation or sample pretreatment steps were required. Satisfactory
results were obtained. Metoprolol recoveries in plasma were determined as 87±2% and 90±4% with PARAFAC and ATLD, respectively.
All RSD values of intra- and interday assays were below 5%.
Figure A three-dimensional plot of EEMs for a plasma sample and metoprolol solution 相似文献
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An HPLC method combined with second-order calibration based on alternating trilinear decomposition (ATLD) algorithm has been developed for the quantitative analysis of levodopa (LVD), carbidopa (CBD) and methyldopa (MTD) in human plasma samples. Prior to the analysis of the analytes by ATLD algorithm, three time regions of chromatograms were selected purposely for each analyte to avoid serious collinearity. Although the spectra of these analytes were similar and interferents coeluted with the analytes studied in biological samples, good recoveries of the analytes could be obtained with HPLC-DAD coupled with second-order calibration based on ATLD algorithm, additional benefits are decreasing times of analysis and less solvent consumption. The average recoveries achieved from ATLD with the factor number of 3 (N = 3) were 100.1 ± 2.1, 96.8 ± 1.7 and 104.2 ± 2.6% for LVD, CBD and MTD, respectively. In addition, elliptical joint confidence region (EJCR) tests as well as figures of merit (FOM) were employed to evaluate the accuracy of the method. 相似文献
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Fluoroquinolones or so-called second-generation quinolones, in particular, ofloxacin (OFL), norfloxacin (NOR), and enoxacin (ENO), with therapeutic advantages possess strongly overlapped fluorescence spectra. In this paper, two strategies were proposed for simultaneous direct determination of OFL, NOR and ENO in plasma by combining fluorescence excitation-emission matrix (EEM) with second-order calibration based on the alternating trilinear decomposition algorithm (ATLD) and parallel factor analysis (PARAFAC). The results showed that both algorithms could solve the problem of serious fluorescence spectral overlapping of the sought-for analytes even in the presence of uncalibrated interferents. However, ATLD has advantages of being insensitive to overestimated component number and fast convergence. The results by using ATLD with an estimated component number of five were reasonably acceptable for clinical analysis. The average recoveries of OFL, NOR and ENO in synthetic samples were 99.7 ± 2.4, 101.5 ± 2.4 and 97.3 ± 3.8%, respectively; the average recoveries of OFL, NOR and ENO in complex plasma were 94.3 ± 2.6, 85.6 ± 3.3 and 103.3 ± 3.0%, respectively. 相似文献
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Yuanbo Gao Tingting Yang Xueli Wang Jizong Chen Yong He 《Journal of polymer science. Part A, Polymer chemistry》2022,60(10):1610-1623
Two series of novel alternating copolyoxamides (PAnT-alt-n2 and PAn2-alt-62) are synthesized via solution/solid-state polycondensation (SSP). The alternating structures are analyzed carefully with 1H NMR and 13C NMR spectra. The melting behaviors, thermal stabilities, crystal structures and crystallinities are systematically evaluated by DSC, TGA and WAXD. The results reveal that these alternating copolyoxamides possess almost perfect alternating chain structures and have high melting temperature (Tm > 270 °C), high crystallinity (Xc > 32%) and high decomposition temperature (T5 > 405 °C) as well as low saturated water absorption (<3.5 wt%), which suggests that they have high potential as engineering plastic of high heat resistant. 相似文献
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Li-Qun Ouyang Hai-Long Wu Jin-Fang Nie Hong-Yan Zou Ru-Qin Yu 《Analytica chimica acta》2009,650(2):160-782
A method using high performance liquid chromatography with photodiode-array detection (HPLC-DAD) coupled with alternating trilinear decomposition (ATLD) algorithm was proposed for simultaneous determination of psoralen and isopsoralen in plasma and Chinese medicine “Xian Ling Gu Bao” capsule (XLGBC). In this paper, the application of ATLD algorithm into traditional chromatographic method can handle this problem that the chromatographic and spectral peaks are heavily overlapped among the analytes and even between the analytes and interferences from the background matrices. A simple improvement of chromatographic condition like mobile phase is not enough to realize effective separation for the two isomeric compounds, especially in the presence of interferences. However, the ATLD algorithm utilized “mathematical separation” instead of partial “physical or chemical separation” to directly determine the spectral profiles of the analytes of interests in complex system. The satisfactory quantification results have been gained with simple mobile phase. In the analysis of real Chinese medicine samples, the accuracy of the concentrations which were obtained by ATLD was also validated by HPLC-MS method. 相似文献
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Haiyan Fu Hedong Li Mei Shao Tianming Yang Xu Zhang Rujing Xu Yujuan Wei Shuhua Chen Chuang Ni Hailong Wu 《中国科学:化学(英文版)》2016,59(7):816-823
A highly sensitive and selective 3D excitation-emission fluorescence method has been proposed to rapidly quantify the combined antidiabetics Repaglinide(Re) and Irbesartan(Ir) in rat and human plasmas with the aid of second-order calibration method based on alternating trilinear decomposition(ATLD) method. Re and Ir with weak fluorescence can be endowed with strong fluorescent property by changing the microenvironment in samples and improving the fluorescence quantum yield by using an appropriate micellar enhanced surfactant. The enhanced excitation-emission matrix fluorescence of Re and Ir can be accurately resolved and can simultaneously attain the optimal concentration even in the presence of a potentially strong intrinsic fluorescence from complex biological matrices, such as rat and human plasmas, by using the ATLD method, which completely exploits the "second-order advantage". The average recoveries of Re and Ir obtained from ATLD with the factor number of 3(N=3) were 101.0%±4.3% and 99.1%±4.1% for rat plasma and 100.5%±5.4% and 97.1%±3.6% for human plasma. Several statistical methods, including Student's t-test, figures of merit, and elliptical joint confidence region, have been utilized to evaluate the accuracy of the proposed method. Results show that the developed method can maintain second-order advantage in simultaneous determinations of the weak fluorescent analytes of interest in different biological plasma matrices. 相似文献
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三维荧光校正法直接测定尿液中的利血平 总被引:1,自引:0,他引:1
利用化学计量学三维数据校正方法中的交替三线性分解算法(ATLD)和自加权交替三线性分解算法(SWATLD), 不经化学分离, 对采用激发-发射矩阵荧光法所得到的三维响应数据阵进行三线性成分分解, 再基于标样已知浓度, 利用简单回归法直接测定尿液中利血平(Reserpine)的含量. 结果表明, 当体系的主要组分数取3时, 两种方法均可迅速、 快捷地得到待测物的浓度, 有效地解决了荧光法定量测定时未知背景及干扰物光谱严重重叠而引起的问题. 相似文献
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Decheng Wan Lianjun Shi Junlian Huang 《Journal of polymer science. Part A, Polymer chemistry》1998,36(16):2927-2931
The spontaneous copolymerization of N-phenylmaleimide (NPMI) (M1) with ethyl α-phenylacrylate (EPA)(M2) were carried out in dioxane at 85°C. A high alternating tendency was observed. The monomer reactivity ratios were r1 = 0.07 ±0.01 and r2 = 0.09 ± 0.02. The maximum copolymerization rate and molecular weight occurs at 70–80 mol% (M1) in feed ratio. The spontaneous alternating copolymerization is considered to be carried out via a contact-type charge transfer complex (CTC) formed between the monomers. Thermogravimetric analyses (TGA) indicate the resulting copolymers have high thermal stability. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 2927–2931, 1998 相似文献
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姜黄素、阿霉素和白藜芦醇对多种恶性肿瘤的治愈皆有一定的疗效,且其联合用药对癌细胞的抑制效果更加显著.本文采用三维激发发射荧光光谱结合基于交替三线性分解(Alternating Trilinear Decomposition,ATLD)算法的化学计量学二阶校正法,同时对血浆样中姜黄素、盐酸阿霉素和白藜芦醇的含量进行了定量分析研究.当量测体系的组分数预估计取4时,ATLD方法解析得到的血浆样中姜黄素、盐酸阿霉素和白藜芦醇的平均回收率分别为(91.4±1.1)%、(104.5±2.8)%和(103.4±4.7)%.实验结果表明,此法能够解决干扰共存和荧光光谱重叠下血浆样中姜黄素、盐酸阿霉素和白藜芦醇的直接、快速、同时定量分析的难题. 相似文献
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E. A. Klop B. J. Lommerts J. Veurink J. Aerts R. R. Van Puijenbroek 《Journal of Polymer Science.Polymer Physics》1995,33(2):315-326
Differential scanning calorimetry and high temperature x-ray diffraction were used to study the perfectly alternating copolymer of ethene and carbon monoxide (polyketone; POKC2). It was found that oriented POK-C2 fibers show a crystalline phase transition at a temperature between 110–125°C with a 10% change in crystalline density. At this temperature, the crystal structure reported recently (POK-α) is transformed to a crystal structure that was reported in the past for room temperature imperfectly alternating polyketone. The latter structure will be designated as POK-β. The influence of chain defects on the crystal structure was studied by synthesizing terpolymers (POK-C2/C3), in which small amounts of propylene-CO units are incorporated into the polymer backbone. The resulting terpolymers differ from the copolymer by the presence of methyl groups randomly distributed along the polyketone backbone chain. Evidence is presented that indicates that the methyl groups are built into the crystal lattice as defects. With more than 5 mole-% propene the terpolymer fibers crystallize exclusively in the β-modification. Below this level the α/β ratio (at room temperature) increases with decreasing amounts of propene. Both as-synthesized and as-spun POK-C2 were found to consist of both POK-α and POK-β; the α/β ratio depends on the method of preparation. Because the drawn POK-C2 fibers studied here consist exclusively of POK-α, the process of spinning and drawing leads to the transformation of unoriented β-rich material into oriented POK-α. © 1995 John Wiley & Sons, Inc. 相似文献
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Yong‐Jie Yu Hai‐Long Wu Chao Kang Yu Wang Juan Zhao Yuan‐Na Li Ya‐Juan Liu Ru‐Qin Yu 《Journal of Chemometrics》2012,26(5):197-208
Although a number of algorithms have established to obtain the well‐known second‐order advantage that quantifies analytes of interest in the presence of interferents, each has associated problems. In this work, for the first time, the optimization procedure of trilinear decomposition has been divided into three subparts, and a novel strategy is developed for assembling the advantages of the alternating trilinear decomposition (ATLD) algorithm, the self‐weighted alternating trilinear decomposition (SWATLD) algorithm, and the parallel factor analysis (PARAFAC) algorithm. The performance of the proposed strategy was evaluated using a simulated data set, a published fluorescence data set together with a new fluorescence data set that simultaneously quantifies procaine and tetracaine in plasma. Results show that the novel method can accurately and effectively estimate the qualitative and quantitative information of analytes of interest. Besides, the resolved profiles are very stable with respect to the number of components as long as the employed number is chosen to be equal or larger than the underlying one. Additionally, the study confirms that better prediction can be obtained by the new strategy when compared with ATLD, SWATLD, and PARAFAC as well as the strategy that employs direct trilinear decomposition method as initial values for PARAFAC. Moreover, the strategy can be directly extended to third‐order or higher‐order data analysis. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
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Toru Doi Akira Akimoto Akikazu Matsumoto Takayuki Otsu 《Journal of polymer science. Part A, Polymer chemistry》1996,34(3):367-373
Radical copolymerization of N-methylmaleimide (MeMI) as well as other N-alkylmaleimides (RMI) and isobutene (IB) was carried out with 2,2′-azobis(isobutyronitrile) as an initiator at 60°C. The initial rate of the copolymerization (Rp) was dependent on the monomer composition and was maximum at the 40 mol % of MeMI in the feed. A solvent effect on the Rp and the monomer reactivity ratio was observed in this copolymerization system, i.e., copolymerization in chloroform produced a higher Rp and an alternating tendency compared with those in dioxane (rMeMI = 0.14, r1B = 0 in chloroform and rMeMI = 0.47, r1B = 0 in dioxane). The alternating copolymer of RMI and IB shows a high glass transition temperature (Tg) and excellent thermal stability, e.g., the Tg and the thermal decomposition temperature (Td) were 152 and 363°C, respectively, for the alternating copolymer of MeMI and IB. Both the Tg and Td increased as the concentration of the MeMI unit in the copolymers increased. Colorless transparent sheets were obtained from press molding the alternating copolymers. They showed excellent mechanical and optical properties. © 1996 John Wiley & Sons, Inc. 相似文献