Spectrofluorimetric Determination of Aflatoxin B1 in Winter Herbal Teas via Magnetic Solid Phase Extraction Method by using Metal–Organic Framework (MOF) Hybrid Structures Anchored with Magnetic Nanoparticles

MIL53(Al)-SiO₂@Fe₃O₄ composite was prepared by co-precipitation route with a typical Stöber synthetic process and ultrasonic-agitation, then subsequently utilized as a multi-component novel sorbent in solid-phase microextraction (SPME) of aflatoxin B1 in winter herbal teas. Microstructural properties of MIL53(Al)-SiO₂@Fe₃O₄ composite was characterized by using Fourier transform infrared (FTIR) spectroscopy, powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) methods, and Brunauer–Emmett–Teller (BET) surface area measurement. The MIL53(Al)-SiO₂@Fe₃O₄ composite was found to be a very effective sorbent in spectrofluorimetric determination of aflatoxin B1 (AFB1) in winter herbal teas via magnetic solid-phase extraction (SPE) route. The proposed method showed a wide linear range from 0.5 to 150 ng/ml, low limit of detection (LOD = 0.5 ng/ml), and an acceptable recovery values (70.7–96.5%) in real samples analysis. This study shows that the suggested method possesses an important potential to use for detecting AFB1 in quality control laboratories.     

荧光光度法测定鸟嘌呤

本文研究表明在碱性介质中,鸟嘌呤可被H2O2氧化(Cu2 作催化剂)生成8-羟基鸟嘌呤,该产物在397 nm处产生强的荧光。据此,建立了一种测定鸟嘌呤的新方法。鸟嘌呤的浓度在2.0×10~(-7)1.0×10~(-5)g·mL-1的范围内与荧光强度有良好的线性关系,检出限为8.0×10~(-8)g·mL-1。该方法简单、快速、灵敏度高,并成功地用于尿样中鸟嘌呤的测定。     

Determination of carbendazim, thiabendazole and fuberidazole using a net analyte signal-based method

The net analyte signal (NAS)-based method HLA/GO, modification of the original hybrid linear analysis (HLA) method, has been used to determine carbendazim, fuberidazole and thiabendazole in water samples. This approach was used after a solid-phase extraction (SPE) step, using the native fluorescence emission spectra of real samples, previously standardized by piecewise direct standardization (PDS). The results obtained show that the modification of HLA performs in a similar way that partial least-squares method (PLS-1). The NAS concept was also used to calculate multivariate analytical figures of merit such as limit of detection, selectivity, sensitivity and analytical sensitivity (γ⁻¹). With this purpose, blanks of methanol and ternary mixtures, with the target analyte at low concentration and the other two ranging according to the calibration matrix, were used, with different results. Detection limits calculated in the last way are more realistic and show the influence of the other components in the sample. Selectivity for carbendazim is higher than the corresponding values for fuberidazole and thiabendazole, whereas sensitivity, as well as the values obtained for their detection limits, are lower for carbendazim, followed by thiabendazole and fuberidazole. Results obtained by modification of HLA vary in the same way that the ones obtained by PLS-1.     

固定波长同步荧光法同时分析2，2′－二羟基联苯和4－羟基联苯

建立了２，２′－二羟基联苯和４－羟基联苯的同时同步荧光分析法。方法简便快速。２，２′－二羟基联苯和４－羟基联苯的线性范围均为０～８μｇ／ｍＬ，检出限分别为６１ｎｇ／ｍＬ和８７ｎｇ／ｍＬ。     

Spectrofluorimetry in organized media coupled to second-order multivariate calibration for the determination of galantamine in the presence of uncalibrated interferences

The present article describes the spectrofluorimetric determination of galantamine, a widely used acetylcholinesterase inhibitor, through excitation-emission fluorescence matrices and second-order calibration. With the purpose of enhancing the fluorescence intensity of this substance, the effect of different organized assemblies was evaluated. Although the interaction of galantamine with different cyclodextrins is weak, it was corroborated that the fluorescence intensity of this pharmaceutical in the presence of α-cyclodextrin is increased by a twofold factor. Among the studied micellar media, the anionic surfactant sodium dodecyl sulfate produced the largest signals for the compound of interest (sixfold enhancement), and was selected as auxiliary reagent for the subsequent determinations. The developed approach enabled the determination of galantamine at the ng mL⁻¹ level without the necessity of applying separation steps, and in the presence of uncalibrated interferences. The applied second-order chemometric tools were parallel factor analysis (PARAFAC), unfolded partial least-squares coupled to residual bilinearization (U-PLS/RBL), and multidimensional partial least-squares coupled to residual bilinearization (N-PLS/RBL). The ability of U-PLS/RBL to successfully overcome spectral interference problems is demonstrated. The quality of the proposed method was established with the determination of galantamine in both artificial and natural water samples.     

Simultaneous determination of hydroquinone, resorcinol, phenol, m-cresol and p-cresol in untreated air samples using spectrofluorimetry and a custom multiple linear regression-successive projection algorithm

In this study, a novel, simple, and efficient spectrofluorimetric method to determine directly and simultaneously five phenolic compounds (hydroquinone, resorcinol, phenol, m-cresol and p-cresol) in air samples is presented. For this purpose, variable selection by the successive projections algorithm (SPA) is used in order to obtain simple multiple linear regression (MLR) models based on a small subset of wavelengths. For comparison, partial least square (PLS) regression is also employed in full-spectrum. The concentrations of the calibration matrix ranged from 0.02 to 0.2 mg L⁻¹ for hydroquinone, from 0.05 to 0.6 mg L⁻¹ for resorcinol, and from 0.05 to 0.4 mg L⁻¹ for phenol, m-cresol and p-cresol; incidentally, such ranges are in accordance with the Argentinean environmental legislation. To verify the accuracy of the proposed method a recovery study on real air samples of smoking environment was carried out with satisfactory results (94-104%). The advantage of the proposed method is that it requires only spectrofluorimetric measurements of samples and chemometric modeling for simultaneous determination of five phenols. With it, air is simply sampled and no pre-treatment sample is needed (i.e., separation steps and derivatization reagents are avoided) that means a great saving of time.     

Studies on the supramolecular interaction between napropamide and β-cyclodextrin by spectrofluorimetry and its analytical application

The supramolecular interaction between N,N-diethyl-2-(1-naphthalenyloxy)propanamide (napropamide) and β-cyclodextrin (β-CD) has been studied by spectrofluorimetry. The results showed that β-CD reacted with napropamide to form an inclusion complex with an association constant of 3.18×10³ l mol⁻¹. The composition of the complex was 1:1 (β-CD:napropamide). Based on the significant enhancement of fluorescence intensity of napropamide in inclusion complex, a spetrofluorimetric method with high sensitivity and selectivity was developed for the determination of napropamide in aqueous solution. Under the optimum conditions, the complex had excitation and emission maxima at 285 and 339 nm, respectively. The linear range of the method was 3.7-1500 ng ml⁻¹ with a detection limit of 1.1 ng ml⁻¹. The proposed method was successfully used to determine napropamide in river water.     

Interaction between pentaethylene glycol n-octyl ether and low-molecular-weight poly(acrylic acid)

The interaction between pentaethylene glycol n-octyl ether (C8E5) and low-molecular-weight poly(acrylic acid) (PAA, M(w)=2000) in aqueous solution has been investigated by various experimental techniques at constant polymer concentration (0.1% w/w) with varying surfactant molality. Spectrofluorimetry, using pyrene as molecular probe, shows (i) the formation of surfactant-polymer aggregates at a surfactant molality (T(1)) lower than the critical micelle concentration (cmc) of C8E5 in water and (ii) the formation of free micelles at a surfactant molality (T(2)) slightly higher than the cmc. Fluorescence quenching measurements indicate that the presence of PAA induces a lowering of the C8E5 aggregation number. Calorimetry confirms spectrofluorimetric evidence; in addition, it shows the presence of weak interactions below T(1) between monomeric surfactant molecules and the polymer chains. Tensiometry shows that, above T(1), only a low fraction of surfactant molecules interact with the polymer and that free micelle formation occurs before polymer saturation. The peculiarities of the interaction between surfactants and low-molecular-weight polymers have been discussed.     

Sensitive determination of enoxacin by its enhancement effect on the fluorescence of terbium(III)-sodium dodecylbenzene sulfonate and its luminescence mechanism

The fluorescence system of enoxacin-Tb³⁺-sodium dodecylbenzene sulfonate (SDBS) was investigated in this paper. The experiments indicated that the fluorescence intensity of Tb³⁺-SDBS was greatly enhanced by enoxacin. Accordingly, a sensitive fluorimetric method for determining enoxacin was established. The fluorescence intensity was measured by a 1-cm quartz cell with an excitation wavelength of 290 nm and an emission wavelength of 545 nm. The enhanced fluorescence intensity of the system (ΔF) showed a good linear relationship with the concentration of enoxacin in the range of 5.0×10⁻⁹ to 2.0×10⁻⁶ mol L⁻¹, its correlation coefficient was 0.9992 and the detection limit (S/N=3) was 2.8×10⁻⁹ mol L⁻¹. The presented method was used to determine enoxacin in real pharmaceutical samples. The luminescence mechanism was also discussed in detail. In the fluorescence system of enoxacin-Tb³⁺-SDBS, SDBS not only acted as the surfactant but also acted as the energy donor.     

氧化还原荧光法测定痕量亚硝酸根

建立了碘化钾与亚硝酸根氧化还还原反应生成游离碘使异硫氰酸荧光素荧光猝灭测定痕量亚硝酸根的新方法,其线性范围为25－100ug/L,回归方程为ΔF＝7．98C－10．5,r=0.990,方法的检测限为12ug/L。本法快速,灵敏,操作简便,用于水样中痕量亚硝酸根的测定,结果良好。