天然结晶辣椒碱的NMR谱研究

用一维¹H NMR谱、¹H-¹H COSY谱和一维¹³C NMR谱、DEPT谱研究辣椒碱分子和二氢辣椒碱分子及其混合物,得到¹H和¹³C的化学位移,采用¹H NMR谱测定天然辣椒碱中辣椒碱和二氢辣椒碱的相对含量.     

外源水杨酸对TMV侵染后辣椒幼苗生理特性的影响

采用烟草花叶病毒侵染辣椒植株,用不同浓度水杨酸处理感病的辣椒植株,测定叶绿素、丙二醛等生理指标,分析其生理生化变化.结果表明：烟草花叶病毒侵染后辣椒叶片叶绿素含量降低、丙二醛含量升高、脯氨酸含量下降、过氧化物酶活性和超氧化物歧化酶活力值明显下降,100μ rnol/L水杨酸处理后生理特性的变化影响较显著,叶绿素含量升高、丙二醛含量降低、脯氨酸含量升高、过氧化物酶和超氧化物歧化酶活性升高,而500μmol/L的水杨酸对辣椒形成胁迫效应.表明外源水杨酸（＜500μmol/L）可以显著提高感染TMV辣椒的抗病性,有利于辣椒幼苗对逆境的适应.     

FAAS测定辣椒中的微量金属元素

采用灰化法处理样品,火焰原子吸收光谱法测定了辣椒中Fe、Zn、Cu、Mn、Mg、Ca、Na元素的含量。结果显示辣椒中这几种元素的含量分别是176.0、26.8、47.2、36.1、1646.7、163.5、1022.4μg/g,RSD为0.3%—3.8%;并分别测定了辣椒籽、皮中这些元素的含量;加标回收率在95.0%—108.1%之间。火焰原子吸收光谱法可以简便、准确地实现辣椒中微量元素的测定。     

辣椒碱与β-环糊精包合物的核磁共振研究

利用核磁共振方法研究了辣椒碱β-环糊精包合物的化学计量比、空间结构信息及其在水溶液中的自扩散系数. 通过测定不同浓度比的辣椒碱和β-环糊精混合溶液的 ¹H NMR数据,绘制Job's曲线,辣椒碱和β-环糊精的Job's曲线均在r=0.5处出现拐点. 同时测定了该包合物的2D ROESY和DOSY谱图,ROESY谱图中NOE交叉信号出现在辣椒碱的H-1~H-8和β-环糊精的H-3′、H-5′、H-6′之间,DOSY测得β-环糊精和辣椒碱形成包合物前后的表观自扩散系数. 结果表明,辣椒碱β-环糊精包合物的主客体分子的化学计量比为1∶1,辣椒碱分子的异丙基端从β-环糊精的宽口端进入疏水腔,其中H-1~H-8部分在空腔内部,包合物的自扩散系数为2.95×10^-10m²/s.     

ICP-AES快速测定云南省部分辣椒果实中的18种元素

采用电感耦合等离子体-原子发射光谱法测定了辣椒中Cu、Na、B、Li、Mn、Ca、Ba、Sr、Zn、Fe、Co、Tl、Al、Ni、Ga、K、Ag、In等18种元素的含量。分析结果的相对标准偏差为0.3%—1.8%,平均回收率在80.00%—116.93%之间。该方法简单、快速、可靠、灵敏度高,且多元素可同时测定,能满足实际样品分析要求。实验表明:辣椒中含有丰富的对人体有益的Ca、Fe、Zn、Mn、Cu、Na等元素,不同品种的辣椒其元素含量存在差异,这种差异与辣椒的基因型有关。用ICP-AES测定辣椒中微量元素对此类资源的充分利用有重要的指导意义。     

荧光光谱法测定大鼠组织中辣椒碱的浓度

在激发波长λex=283nm,发射波长λem=320nm下,采用荧光光谱法测定大鼠的几种组织中辣椒碱的浓度.辣椒碱的荧光值基本不受各组织的影响;线性范围为0.01-0.8μg/mL,检出限为5ng/mL;平均回收率均大于90%,RSD均小于7%.该方法快速、简便,适用于辣椒碱的体内研究.     

HPLC-DAD法测定辣椒及其制品中苏丹红Ⅰ的含量

二极管阵列检测器(DAD),高效液相色谱法定性定量测定辣椒产品中的苏丹红Ⅰ.方法具有良好的稳定性和重现性,切实可行.分析结果表明,在我国的辣椒及其制品中未曾检测到该物质的存在.     

辣椒红素分子体外氧化防御反应UV-Vis及FTIR光谱特征分析

采用紫外-可见光谱(UV-Vis)和傅里叶变换红外光谱(FTIR)法分析辣椒红素在外源活性氧·O-₂,H₂O₂和·OH以及在POD,CAT和LOX防御体系中的结构变化特征。结果表明,外源活性氧处理后辣椒红素最大紫外-可见光吸收峰均出现蓝移现象,其中·O-₂和·OH处理后产物FTIR谱峰数减少,峰强变弱,峰形变宽;与色素分子中的羰基和环外烯基发生氧化反应生成烷基和羟基,·OH对色素分子CC具有加成作用;H₂O₂处理后色素特征峰和强势峰均向低波数位移,产物中含环氧醚基团;在H₂O₂+CAT/POD防御体系中辣椒红素UV-Vis和FTIR光谱特征无明显变化;在亚油酸+LOX体系中色素分子结构发生断裂,产物不含羰基。可见活性氧处理及在LOX底物体系中,辣椒红素分子反应前后UV-Vis和FTIR等光谱特征发生明显变化,色素分子中长烯链断裂,大共轭体系缩短或被破坏,分子中的共轭双键和羰基等发色基团改变,最终生成醇类或醚类等小分子无色物质;而防御酶CAT和POD能减少活性氧对辣椒红素分子的破坏作用。研究结果丰富完善了辣椒色素理论,同时为其开发利用提供了有价值的技术参考依据。     

辣椒素的纯化及分析

使用活性炭纯化辣椒碱粗提物,RP-HPLC定量测定辣椒素样品中主要成分。在优化条件下得到辣椒素提取物纯度为97．2％。     

红外光谱结合化学计量学对朝天椒和涮涮辣的研究

本文利用红外光谱结合主成分(PCA)和偏最小二乘法判别分析(PLS-DA)研究了朝天椒(簇生椒)和涮涮辣。测试了2种辣椒60个样品的红外光谱,对光谱范围1800~950cm-1做二阶导数处理,发现在该区间存在着明显的差异,利用该区间二阶导数光谱数据进行主成分分析和偏最小二乘法,结果表明PCA和PLSDA都能很好的区别两种辣椒,其中主成分的正确率为100%,偏最小二乘法在隐含潜含变量为12个时其正确率最好,朝天椒的正确率为86.7%,涮涮辣的正确率为93.3%。结果表明小波变换结合PCA和PLS-DA用于傅里叶变换红外光谱技术中能够准确地识别朝天椒和涮涮辣,为区分不同品种的辣椒提供快速和有效的方法。     

HPLC-DAD法测定辣椒及其制品中苏丹红的含量

建立了应用高效液相色谱测定辣椒粉及其少量含油制品中的苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ含量的检测方法.采用Symmetry C18反相色谱柱(3.9mm×150mm,5μm),流动相为乙腈醋酸溶液(V乙磷:Vo.1%醋酸＝7∶1),等度洗脱,流速1.0mL/min;柱温30℃;检测波长230nm.在选定色谱条件下,苏丹红Ⅰ、Ⅱ、Ⅲ、...     

苏丹红系列染料在有机溶液中的紫外-可见光谱研究

研究了苏丹红Ⅰ、苏丹红Ⅲ和苏丹红Ⅳ在非极性溶剂石油醚和极性溶剂乙腈及乙腈-水混合溶液中的紫外-可见光谱特征。在极性溶剂中苏丹红系列的可见区特征吸收峰比在非极性溶液中略有红移;在乙腈-水混合溶液中,苏丹红Ⅰ的特征吸收峰比在乙腈溶剂中红移,最大红移达13 nm,吸收强度最大增幅为34.5%;苏丹红Ⅲ的特征吸收峰红移8 nm,吸收强度增幅为11%;苏丹红Ⅳ的特征吸收峰先红移后蓝移,吸收强度增幅数仅为2.5%。造成这一变化的原因是在乙腈-水混合溶液中,苏丹红Ⅰ, Ⅲ, Ⅳ分子内氢键被破坏,扩大了π键离域范围所致。     

Using a 1,8-diamino naphthalene–copper (II) system as a turn-on fluorescence probe for detecting Sudan I

An easy-to-use fluorescence probe for detecting Sudan I was developed. The probe detects Sudan I because Sudan I and 1,8-diamino naphthalene competitively interact with copper (II). Copper (II) effectively quenches the fluorescence of 1,8-diamino naphthalene because the 1,8-diamino naphthalene interacts with copper (II) and forms a 1,8-diamino naphthalene–copper (II) complex. Adding Sudan I causes the fluorescence of the system to be recovered because the Sudan I removes copper (II) from the 1,8-diamino naphthalene–copper (II) complex, liberating the 1,8-diamino naphthalene. The displacement of 1,8-diamino naphthalene by Sudan I gives a high fluorescence recovery efficiency. Under optimal conditions, the fluorescence intensity F achieved when Sudan I was added had a good linear relationship (R²?=?0.999) with the Sudan I concentration over the range 0–4.6?µM. The Sudan I detection limit was 0.032?µM. The method offers a new way of quantitatively determining Sudan I.     

Highly sensitive electrochemical sensor for Sudan I based on graphene decorated with mesoporous TiO2

A sensor for the highly sensitive determination of Sudan I based on the amplified electrochemical response of mesoporous TiO₂-decorated graphene (GN–TiO₂) was fabricated. The nanoparticles of TiO₂ arrayed densely and uniformly on the GN sheets, as confirmed by field emission scanning electron microscopy and transmission electron microscopy images. The electrochemical behavior of Sudan I at this sensor was studied in detail, showing that this sensor exhibited electrocatalytic activity for the oxidation of Sudan I because of the significant peak current enhancement and the lowering of oxidation overpotential. Furthermore, the experimental parameters including supporting electrolyte, volume of GN–TiO₂ suspension on electrode surface, accumulation potential, and time were optimized and the electrochemical reaction mechanism of Sudan I on this sensor was investigated. The linear range is from 3.3 nM to 0.66 μM, and the limit of detection is estimated to be 0.60 nM. At last, the sensor was used to determine Sudan I in food sample extracts, which are in good agreement with the results obtained by chromatographic method.     

Phytochemicals in Capsicum oleoresin from different varieties of hot chilli peppers with their antidiabetic and antioxidant activities due to some phenolic compounds

Due to its wide use in nutritional therapy, a capsicum oleoresin extraction from hot chilli pepper was optimized using ultrasound assisted extraction. Under optimal conditions, a 0.1 g sample in 10 mL of a 20% water in methanol solution was extracted at 50 °C for 20 min to remove phytochemicals consisting of oleoresin, phenolics, carotenoids, flavonoids, capsaicinoids (pungency level), reducing sugars. Antioxidant and antidiabetic activities of the crude extracts from 14 chilli pepper varieties were examined. The antioxidant and antidiabetic activities of some phenolic compounds were also tested individually. The results showed that these chilli pepper samples are a rich source of phytochemicals with antioxidant and antidiabetic activities. High antioxidant activity of the extracts was evaluated using the 2,2-diphenyl-1-picrylhydrazyl, N,N-dimethyl-p-phenylenediamine dihydrochloride, 2,2′-azino-bis(3-ethylbenzothiazolin-6-sulfonic acid) and ferric ion reducing antioxidant power assays. The crude extracts had a lower level of sugars induced by the inhibitory effect of α-amylase activity. Thus, their enzymatic inhibitory effect might have resulted from a synergism among the phytochemicals concerned. Therefore, a diet with this type of food may have beneficial health effects.     

The study on the nonlinear optical response of Sudan I

The nonlinear optical properties of Sudan I were investigated by a single beam Z-scan technique. The Sudan I ethanol solution exhibited large nonlinear refractive indices under both CW and pulse laser excitations. The nonlinear refractive indices of Sudan I were in the order of ?10^?8 cm²/W under CW 633 nm excitation and ?10^?6 cm²/W under CW 488 nm excitation, respectively. Under the excitation of a pulse 532 nm laser, the nonlinear refractive index n₂ was calculated to be 1.19 × 10^?14 cm²/W. It was discussed that the mechanism accounting for the process of nonlinear refraction was attributed to the laser heating for the CW laser excitation and the electronic effect for the pulse excitation. Moreover, the second hyperpolarizability of Sudan I was also estimated in this paper.     

Highly Selective and Sensitive Benzimidazole Based Bifunctional Sensor for Targeting Inedible Azo Dyes in Red Chilli,Red Food Color,Turmeric Powder,and Cu(Ii) in Coconut Water

In this study, a simple Benzimidazole based bifunctional chemosensor 4-(2-(3,4-dimethoxyphenyl)-1H-benzo[d]imidazol-6-yl) benzene-1,2-diamine, L was synthesized and characterized. The sensor proved to be selective and sensitive towards detecting banned azo dyes Sudan Dye I, II, and Metanil Yellow via fluorescence turn-off response. The proposed mechanism of fluorescence quenching was the inner filter effect. LODs for Sudan I, II, and Metanil Yellow were found to be 0.009 µM, 0.012 µM, and 0.0073 µM, respectively. The developed chemosensor also showed a colorimetric response towards Cu (II) ions via an apparent color change from yellow to pink. LOD for Cu (II) ions was found to be 1.2 µM. The synthesized benzimidazole based bifunctional chemosensor was adequately tested to determine Sudan I in Red chili powder and red Food color samples, Metanil yellow in turmeric powder, and Cu(II) packaged coconut water.

     

Experimental and ab initio DFT calculated Raman spectrum of Sudan I,a red dye

The red dye Sudan I was investigated by Raman spectroscopy using different excitation wavelengths (1064, 532 and 244 nm). A calculation of the Raman spectrum based on quantum mechanical ab initio density functional theory (DFT) was made using the RB3LYP method with the 3‐21G and 6‐311 + G(d,p) basis sets. The vibrations in the region 1600–1000 cm⁻¹ were found to comprise various mixed modes including in‐plane stretching and bending of various C C, N N, C N and C O bonds and angles in the molecule. Below ∼900 cm⁻¹, the out‐of‐plane bending modes were dominant. The central hydrazo chromophore of the Sudan I molecule was involved in the majority of the vibrations through NN and C N stretching and various bending modes. Low‐intensity bands in the lower wavenumber range (at about 721, 616, 463 and 218 cm⁻¹) were selectively enhanced by the resonance Raman effect when using the 532 nm excitation line. Comparison was made with other azo dyes in the literature on natural, abundant plant pigments. The results show that there is a possibility in foodstuff analysis to distinguish Sudan I from other dyes by using Raman spectroscopy with more than one laser wavelength for resonance enhancement of the different bands Copyright © 2011 John Wiley & Sons, Ltd.     

Stochastic resonance is applied to quantitative analysis for weak chromatographic signal of Sudan I

Based on the algorithm of stochastic resonance, a new method improved the signal-to-noise ratio (SNR) of weak chromatography signal remarkably. An excellent quantitative relationship can be obtained between concentration and weak chromatography signals of Sudan I which was embedded in the noise background.     

利用AAO模板制备SERS基底检测SudanⅠ

通过模板法制备大面积、可控的、可重复的、热点集中的金纳米结构阵列,并在纳米结构阵列上通过化学修饰分子,吸附更多苏丹红Ⅰ分子至金纳米的SERS增强区域,实现其高灵敏的表面增强拉曼分析检测。以多孔阳极氧化铝为模板,通过真空蒸镀金,约200 nm厚度,复制氧化铝的孔洞结构,用碱液将氧化铝模板腐蚀去除,可得到氧化铝模板的互补结构,即大面积的、均匀的金半球纳米结构阵列。在金纳米结构阵列上修饰十二硫醇,硫醇巯基端与纳米金相结合,碳链端自组装形成非极性的疏水环境,疏水环境可以捕获苏丹红Ⅰ分子,使其吸附至纳米金结构表面的SERS增强区域,实现苏丹红Ⅰ的SERS检测。由于SERS基底表面的金半球纳米结构均匀、规整,在激光光斑的区域内,苏丹红Ⅰ的SERS信号均匀、稳定,可以对苏丹红Ⅰ进行定量分析。苏丹红Ⅰ的拉曼峰强度对数与浓度对数之间呈线性关系,线性相关系数达0.99,线性范围为5×10-4～10-7mol·L-1,回收率范围77%～117%。此方法的检测限可达到4×10-8mol·L-1,与国标的高效液相色谱的检测限相当。