微波消解-液相色谱-原子荧光光谱联用(LC-AFS)法测定稻米样品中砷形态

建立了稻米中4种砷元素形态的液相色谱-原子荧光光谱联用法(LC-AFS),样品用0.15mol/L的硝酸溶液微波提取50min,提取液经离心分离后,采用Hamilton PRP-X100色谱柱,45mmol/L KH2PO4-5mmol/L Na2HPO4缓冲液为流动相,砷形态4个组分能够在7min内达到基线分离,且无需调pH。优化了氢化物发生条件,使用了更低浓度的载流和还原剂。方法学实验结果表明,各组分在2~10ng/mL范围内线性关系良好,相关系数为0.9988~0.9998,各组分的检出限分别为0.29 ng/mL、0.47 ng/mL、0.62 ng/mL和1.16 ng/mL；各组分峰面积的相对标准偏差均低于3.11%；加标回收率为85.3%～112.8%；对稻米标准物质的分析测定结果表明该方法定值准确。最后,与GB 5009.11-2014中使用的提取及测量条件进行对比,表明该方具备法快速、环保、高效的特点。     

Determination of macrolides in livestock excreta by syringe purification coupled with liquid chromatography tandem mass spectrometryEI北大核心CSCD

A method of syringe-dispersive solid-phase extraction combined with ultrahigh performance liquid chromatography with tandem mass spectrometry for the simultanous determination of 10 macrolides in manurebased fertilizers was developed. After extraction with methanol and acetonitrile,the extracts were purified by insyringe dispersion solid-phase extraction in syringes pre-filled with 60 mg PSA and 30 mg C18. The resulted extracts were further separated by a BEH C18 column,detected by multiple reaction monitoring in electrospray positive ion mode,and quantified by matrix-matched external standard method. The results showed that the recoveries of the target compounds ranged from 70% to 110% at three spiked levels（10,30,and 50 μµg/kg）with the relative standard deviations ranged from 1.4% to 12%. The limits of detection and quantification were 0.57 1.75 and 2.77-5.40 μµg/kg,respectively. This method was suitable for the simultaneous determination of residual macrolides in organic fertilizers. © 2023, Youke Publishing Co.,Ltd. All rights reserved.     

Experimental strategy of the spectrophotometric approach using freeze-drying for PO43− determination in frozen and chilled chickens in the Saudi Arabia market

Herein, an efficient analytical method based on an extraction protocol was developed and validated for the spectrophotometric detection of phosphate (PO₄^3?) in chilled and frozen chicken samples. The preparation was a very simple sample that included freeze-drying, extraction with acidified amino acids and filtration of the final extract prior to spectrophotometric analysis. FT-IR spectrum of CS1 was confirmed that the selected solvent has successfully extracted PO₄^3? from the chilled chicken sample. Analytical performances were assessed in chilled of one of the merchant species and showed good recoveries with relative standard deviations (RSD) below 2%. The analytical validation parameters of the method in terms of limit of quantification (LOQ) and detection (LOD) were calculated and found to be 0.10 and 0.032 mg/L, respectively. This protocol has been effectively applied to PO₄^3? determination in chicken samples collected from Saudi supermarkets (Northern KSA), and PO₄^3? in all frozen samples was detected at high mg/kg levels ranging from 2.11 × 10⁴ to 2.90 × 10⁴ mg/kg, while in limit levels of PO₄^3? concentration were detected in the chilled samples except chilled sample 1 (CS1), which was 2.22 × 10⁴ mg/kg. The extraction and determination protocol suggested that this developed method could be validated for routine monitoring of PO₄^3? in food quality control laboratories and safety monitoring.     

三丁基氧化膦-离子液体体系萃取UO2(NO3)2的机理和选择性

The extraction of UO₂(NO₃)₂ from aqueous solution was investigated using trioctylphosphine oxide (TOPO) and tributylphosphine oxide (TBPO) in ionic liquids (ILs) (C_nmimNTf₂, n=2, 4, 6, 8). A third phase was formed in the TOPO-C₂mimNTf₂ and TOPO-C₄mimNTf₂ extraction systems, whereas the extracted species of TBPO-C_nmimNTf₂ (n=2, 4, 6, 8) were well soluble in all ILs. The influence of the concentrations of the extractant, nitric acid, and salt on the extraction efficiency was also investigated. Adding HNO₃ to the aqueous phase decreased the extraction efficiency. The effect of salt indicates the presence of a cation-exchange mechanism in the extraction. The addition of NO₃ - in the aqueous phase increased the extraction efficiency of U, which indicates that NO₃ - participates in the extraction. Selective extraction research indicates that TBPO-C₄mimNTf₂ exhibits good selectivity for U at low acid concentration despite the significant extraction efficiency on Zr at high acid concentration. After removing U, TBPO-C₄mimNTf₂ still showed high selectivity for Nd at low acid concentration. We also confirmed the difference of the extraction mechanisms among TBPO-C_nmimNTf₂ by quantitative measurement of NNO₃ - in ILs, electrospray ionization mass spectroscopy (ESI- MS), and UV spectroscopy. There are two extraction species (UO₂(TBPO)₃(NO₃)⁺ and UO₂(TBPO)₃²⁺) and the proportion of UO₂(TBPO)₃(NO₃)⁺ increases from C₂mimNTf₂ to C₈mimNTf₂.     

杂多酸离子液体催化燃油萃取氧化脱硫性能研究

本文首次将一系列含有不同酸性咪唑阳离子和不同杂多酸阴离子的杂多酸离子液体[C4mim]3PW12O40、[COOH-Cmim] 3PW12O40、[SO3H-C3mim]3PW12O40、[SO3H-C3mim]3PMo12O40和[SO3H-C3mim]4 SiW12O40作为催化剂,乙腈为萃取剂,H2O2为氧化剂,用于催化含二苯并噻吩、苯并噻吩及噻吩模型油的萃取氧化脱硫研究中.实验结果显示,杂多酸离子液体催化燃油脱硫性能不仅与阳离子的酸性强弱有关,而且与阴离子结构密切相关.阳离子的催化活性顺序为:[SO3H-C3mim]+＞[COOH-Cmim]+＞[C4mim]+;阴离子的催化活性顺序为PW12O403-＞ PMo12O403-＞ SiW12O404-.其中[SO3H-C3 mim]3 PW12O40催化活性最高,在60℃反应40min的条件下,二苯并噻吩的转化率约为100％,催化不同硫化物的转化率为:二苯并噻吩＞苯并噻吩＞噻吩.此外,该杂多酸离子液体循环使用5次催化活性仅略有下降.     

破乳诱导萃取-电感耦合等离子体质谱法测定柴油中的锰、铁和铅

采用破乳诱导萃取的前处理方法,结合电感耦合等离子体质谱技术(ICP-MS),测定了柴油中的锰、铁和铅元素。首先将样品和表面活性剂溶液(Triton X-114)混合形成稳定的油包水乳液,以硝酸作萃取剂充分萃取柴油中的锰、铁和铅,然后将乳液离心破乳分层,采用ICP-MS内标法测定酸性水相中的锰、铁和铅。3种元素的检出限(3S/N)在0.008~0.083μg·L-1之间,测定下限(10S/N)在0.027~0.28μg·L-1之间。应用该方法对柴油中金属元素进行测定,加标回收率在94.9%~106%之间,相对标准偏差(n=6)在0.66%~2.2%之间。     

结合区域提取和改进卷积神经网络的水下小目标检测

针对水下小目标信息量有限而难以提取有效特征导致的检测性能不佳问题,提出了一种结合区域提取和融合Hu矩特征的改进卷积神经网络水下小目标检测方法。该方法包含区域提取和分类两个步骤。首先以马尔可夫随机场分割算法为基础进行区域提取,对潜在目标定位的同时降低伪目标对后续分类的干扰;然后提取潜在目标区域的Hu矩特征并融入卷积神经网络,形成一种形状特征表征能力更强的改进卷积神经网络用于分类。声呐实测数据处理结果表明,该方法可以有效提升对水下小目标的发现概率和正确报警率,与其他目标检测方法相比,该方法具有更好的检测性能和泛化性。     

Ultrasound-assisted polysaccharide extraction from Cercis chinensis and properites,antioxidant activity of polysaccharide

The purpose of the study was to improve the extraction of polysaccharide from the leaves of Cercis chinensis Bunge using ultrasound, and compare the difference between boiling and ultrasound extraction in terms of polysaccharide content, monosaccharide compounds, and evaluate how the factors affected the bioactivity. The best conditions, according to the single factor experiments and the Box-Bohnken design (BBD), were an intensity of ultrasound of 180 W, duration of extraction of 40 min, proportion of water to material of 15:1 (g/g), and a higher polysaccharide yield of 20.02 ± 0.55 (mg/g) than in boiling extraction (16.09 ± 0.82 mg/g). The antioxidative experiment suggested the polysaccharide by ultrasound exhibited higher DPPH, hydroxyl radical scavenging capacities, and reducing power at 1.2–1.4 mg/mL, which was superior to the boiling polysaccharide. Further analysis showed that the ultrasonic purified polysaccharides like Gla, N-Glu, and GluA contained more total sugar and uronic acids than the boiling method did. This may indicate that the ultrasonic isolation of the polysaccharides increase the antioxidant activity of the polysaccharides.     

Rapid and label-free classification of pathogens based on light scattering,reduced power spectral features and support vector machine

The rapid identification of pathogens is crucial in controlling the food quality and safety. The proposed system for the rapid and label-free identification of pathogens is based on the principle of laser scattering from the bacterial microbes. The clinical prototype consists of three parts: the laser beam, photodetectors, and the data acquisition system. The bacterial testing sample was mixed with 10 mL distilled water and placed inside the machine chamber. When the bacterial microbes pass by the laser beam, the scattering of light occurs due to variation in size, shape, and morphology. Due to this reason, different types of pathogens show their unique light scattering patterns. The photo-detectors were arranged at the surroundings of the sample at different angles to collect the scattered light. The photodetectors convert the scattered light intensity into a voltage waveform. The waveform features were acquired by using the power spectral characteristics, and the dimensionality of extracted features was reduced by applying minimal-redundancy-maximal-relevance criterion (mRMR). A support vector machine (SVM) classifier was developed by training the selected power spectral features for the classification of three different bacterial microbes. The resulting average identification accuracies of E. faecalis,E. coli and S. aureus were 99%, 87%, and 94%, respectively. The overall experimental results yield a higher accuracy of 93.6%, indicating that the proposed device has the potential for label-free identification of pathogens with simplicity, rapidity, and cost-effectiveness.     

Organic pollutants adsorbed on microplastics: Analytical methodologies and occurrence in oceans

The massive use of plastics in several products has generated microplastic debris worldwide. Besides their negative effect on marine organisms by ingestion, microplastics are a contamination vector due to their capacity to transport organic pollutants around our planet. To evaluate the magnitude of this issue, it is necessary to know what kinds of contaminants are adsorbed on microplastics, as well as their concentrations. In order to assess the adsorption and desorption of pollutants from microplastics, effective and reliable extraction procedures are required. In this overview, literature reports, in which extraction, separation and determination methods have been applied to analyse the organic pollutants adsorbed on microplastics, are revised and discussed. Furthermore, the worldwide occurrence of organic compounds found on microplastics in oceans is reviewed and the results obtained from different geographical areas and their global distribution trends are compared. Priority organic pollutants, such as polycyclic aromatic hydrocarbons, hexachlorocyclohexanes, polychlorinated benzenes, perfluoroalkyl substances or bisphenol analogues, have been widely found on microplastic samples. Future research that focuses on different kinds of emerging pollutants is required.