Simultaneous determination of triazine herbicides in rice by high-performance liquid chromatography coupled with high resolution and high mass accuracy hybrid linear ion trap-orbitrap mass spectrometry

A method was developed for the simultaneous determination of 10 triazine herbicides (cyanazine, simazine, simetryn, metribuzin, atrazine, ametryn, terbuthylazine, prometryn, terbutryn, and dimethametryn) in rice samples by high resolution and high mass accuracy hybrid linear ion trap-Orbitrap mass spectrometer. After extraction with acetonitrile and evaporation, the herbicides were redissolved in n-hexane and purified on a Florisil solid-phase extraction column. All compounds were separated within 12 min, producing more than 11 data points for each herbicide and high mass accuracy quantified ions which the mass errors of absolute value were less than 1.9 ppm in pure solution and 2.1 ppm in the matrix-matched standards solution. The method was validated in terms of the limits of detection and the limits of quantification. The linearity was satisfactory, with a correlation coefficient of >0.9975. Precision and recovery studies were evaluated at three concentration levels for Japonica, Indica, and Glutinous rice matrix. The mean recoveries obtained for all analytes in spiked Xiushui 03, Liangyoupeijiu, and Taihunuo rice samples were 83.3–99.0%, 82.0–99.7%, and 84.2–99.4%, respectively, with relative standard deviation in range 1.7–10.6%, 1.2–10.7%, and 1.9–11.6% for spiked rice samples, respectively. The intra-day precision (n = 5) for the 10 herbicides in rice samples spiked at an intermediate level was between 2.8% and 7.9%, and the inter-day precision over 10 days (n = 10) was between 5.5% and 15.9%.     

A general copper powder-catalyzed Ullmann-type reaction of 3-halo-4(1H)-quinolones with various nitrogen-containing nucleophiles

3-(N-Substituted) 4(1H)-quinolinones were synthesized using the copper-catalyzed Ullmann C-N bond forming strategy in moderate to quantitative yields. Starting from 3-halo-4(1H)-quinolones, various nucleophiles including amides, lactams, sulfonamides and NH-containing azoles have been used successfully. In all cases, the reactions take place rapidly in toluene and proceed by using copper powder as a catalyst, DMEDA as a ligand and K(2)CO(3) as a base. In addition, other related heterocycles such as 3-bromoquinolin-2(1H)-ones, 3-bromocoumarin, and 3,5-dibromo-2-pyridone show good to very high reactivity with various nucleophiles under our Cu/DMEDA catalyst system.     

Characterizations of iron-rich clay modified electrodes and their applications in optical recognition

Optical recognition was studied with modified electrodes based on iron-rich clays. According to energy-dispersive X-ray spectroscopy (EDX), several clay minerals including montmorillonite K10 (mont. K10) contain a lot of iron. Cyclic voltammetry suggested that electrochemically active iron species exist in most iron-rich clays and are likely to reside at different sites. The associated electrochemical activity is strongly pH-dependent and photosensitive. Under UV irradiation (λ ≤ 420 nm), these iron species were activated, and a pronounced photocurrent resulted. When these electrodes were flow-injected with 2-pyridylcarboxylic acids (λ_ab,max = 260 nm), the originally monotonic photocurrent could be modulated into a more recognizable a.c. pattern and the 260 nm optical signal became distinguishable. The photoresponse was highly reproducible, and the response time (t₉₀) was less than 10s.     

多属性决策的组合赋权法

鉴于多属性决策问题中主观赋权法和客观赋权法各有其自身固有的特点，本文依据优化理论提出一种集成方法确定属性权重，该方法既充分利用客观信息，又反映决策者的主观偏好，从而使确定的属性权重更加合理、实用．     

Structure of Cytochromec and Its Platinum-modified Derivatives by Fourier Transform Infrared Spectroscopy

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新重丰中子同位素239Pa

用50MeV/u ¹⁸O离子同天然铀靶反应产生了新重丰中子同位素²³⁹Pa.用放射化学法从反应产物中分离Pa活性,通过观测²³⁹Pa及子体²³⁹U衰变所得到的结果显示:首次合成和鉴别了新重丰中子核素²³⁹Pa,并测定出²³⁹Pa的半衰期为106±30min.     

禽肉中克球酚气相色谱微量快速测定法

对禽肉样品中克球酚药物残留采用微量化学法技术，以甲醇提取，氧化铝、阴离子树脂交换柱净化，乙酰化后，进行ＧＣ－ＥＣＤ毛细管色谱测定。经对肉鸡、填鸭、饲养山鸡进行添加回收率试验，方法回收率为８５．７％～９４．４％，变异系数为３．８％～７．７％，最低检出限为２．０ｎｇ／ｇ。     

175Er的衰变纲图

用14MeV中子照射天然Yb靶,通过¹⁷⁶Yb(n,2p)¹⁷⁵Er反应产生了新的重丰中子同位素¹⁷⁵Er,借助X-γ,γ-γ符合测量方法,首次鉴别出了¹⁷⁵Er,并测得其半衰期为(1.2±0.3)min.同时还观察到了¹⁷⁵Er衰变所发射的8条新γ射线,建立了¹⁷⁵Er的部分γ衰变纲图,从中指定了¹⁷⁵Tm的一个基态转动带.     

金水六君煎胶囊多指标成分分析

采用薄层扫描法、紫外分光光度法分别对金水六君煎胶囊中有祛痰作用的β-谷甾醇和总生物碱进行含量测定。 β-谷甾醇平均回收率为 10 0 .6 % (n=5 ) ,RSD为 2 .77% ;总生物碱平均回收率为 98.4 %(n=5 ) ,RSD为 2 .16 %。该方法简单快速、结果准确、精密度较高 ,可用于该制剂的质量控制。