Determination,residue and risk assessment of trifloxystrobin,trifloxystrobin acid and tebuconazole in Chinese rice consumption

A simple and rapid analytical method for the detection of trifloxystrobin, trifloxystrobin acid and tebuconazole in soil, brown rice, paddy plants and rice hulls was established and validated by liquid chromatography with tandem mass spectrometry. Acceptable linearity (R² > 0.99), accuracy (average recoveries of 74.3–108.5%) and precision (intra- and inter-day relative standard deviations of 0.9–8.8%) were obtained using the developed determination approach. In the field trial, the half-lives of trifloxystrobin and tebuconazole in paddy plants were 5.7–8.3 days in three locations throughout China, and the terminal residue concentrations of trifloxystrobin and tebuconazole were <100 and 500 μg/kg (maximum residue limits set by China), respectively, at harvest, which indicated that, based on the recommended application procedure, trifloxystrobin and tebuconazole are safe for use on rice. The risk assessment results demonstrated that, owing to risk quotient values of both fungicides being <100%, the potential risk of trifloxystrobin and tebuconazole on rice was acceptable for Chinese consumers. These data could provide supporting information for the proper use and safety evaluation of trifloxystrobin and tebuconazole in rice.     

Fabrication and characterization of cellulose nanoparticles from maize stalk pith via ultrasonic-mediated cationic etherification

In this study, parenchyma cellulose, which was extracted from maize stalk pith as an abundant source of agricultural residues, was applied for preparing cellulose nanoparticles (CNPs) via an ultrasound-assisted etherification and a subsequent sonication process. The ultrasonic-assisted treatment greatly improved the modification of the pith cellulose with glycidyltrimethylammonium chloride, leading to a partial increase in the dissolubility of the as-obtained product and thus disintegration of sheet-like cellulose into nanoparticles. While the formation of CNPs by ultrasonication was largely dependent on the cellulose consistency in the cationic-modified system. Under the condition of 25% cellulose consistency, the longer sono-treated duration yielded a more stable and dispersible suspension of CNP due to its higher zeta potential. Degree of substitution and FT-IR analyses indicated that quaternary ammonium salts were grafted onto hydroxyl groups of cellulose chain. SEM and TEM images exhibited the CNP to have spherical morphology with an average dimeter from 15 to 55 nm. XRD investigation revealed that CNPs consisted mainly of a crystalline cellulose Ι structure, and they had a lower crystallinity than the starting cellulose. Moreover, thermogravimetric results illustrated the thermal resistance of the CNPs was lower than the pith cellulose. The optimal CNP with highly cationic charges, good stability and acceptable thermostability might be considered as one of the alternatively renewable reinforcement additives for nanocomposite production.     

Investigations on association schemes with elementary abelian thin residue

In this paper, we give a new class of association schemes whose thin residues are isomorphic to an elementary abelian $p$-group of order $p^2$. We then study the automorphism groups of these schemes and determine whether these schemes are schurian.     

Simultaneous determination of eight short‐chain aliphatic amines in drug substances by HPLC with diode array detection after derivatization with halonitrobenzenes

Short‐chain aliphatic amines are a class of hazardous impurities in drug substances. A simple method, involving derivatization followed by high‐performance liquid chromatography with diode array detection, has been developed for residue determination of eight aliphatic amines simultaneously in drug substances. Different halonitrobenzenes derivatization reagents were systematically compared. As a result, 1‐fluoro‐2‐nitro‐4‐(trifluoromethyl)benzene was selected since the derivatization effectively shifted the absorption wavelength to the visible region (400–450 nm), where most drug substances, impurities and even the derivatization reagent absorb very weakly. Due to the redshift effect, interference was minimized and adequately low limits of quantitation were reached (0.24–0.80 nmol/mL). Moreover, the derivatization reaction was readily carried out in dimethyl sulfoxide at room temperature for 1 h using N ,N‐diisopropylethylamine as catalyst to achieve the highest yield. Without any pre‐treatment, the derivatives were analyzed by high‐performance liquid chromatography with diode array detection. The high stability of the derivatives within 24 h at room temperature (RSD<1.04%) further facilitated the simultaneous preparation and consecutive analysis of quantities of samples. Finally, the proposed method was successfully applied for residue determination of eight aliphatic amines simultaneously in eight drug substance samples. This study could be helpful for the routine analysis and residue control of aliphatic amines in drug substances.     

Deep eutectic solvent-based modified quick,easy, cheap,effective, rugged,and safe extraction combined with solidification of floating organic droplet-dispersive liquid–liquid microextraction of some pesticides from canola oil followed by gas chromatography analysis

Herein, a modified quick, easy, cheap, effective, rugged, and safe extraction was developed based on deep eutectic solvent for the extraction of several pesticides from canola oil samples. In this work, first, different sorbents were selected to remove the sample interferences, and the composition of the sorbents was optimized by simplex centroid design. The extracted analytes were more concentrated by solidification of floating deep eutectic solvent droplet-dispersive liquid–liquid microextraction. Low limits of detection (0.15–0.23 ng/g) and quantification (0.49–0.76 ng/g), high extraction recoveries (74–87%) and enrichment factors (224–263), and good repeatability (relative standard deviation equal to or less than 5.1 and 4.7% for intra- and interday precisions, respectively) were achieved using the proposed method. The suggested approach was used for the quantification of the analytes in different canola oil samples. Additionally, the effects of microwave irradiations exposure and sonication in decontamination of the samples were evaluated. In this method, there was no need for centrifugation and toxic solvents. Also, effective extraction of the analytes and minimizing interferences were achieved through the use of various sorbents.     

Residue valorization: Preparation of recyclable organic amine adsorbent using laterite residue

This study focuses on exploiting the main component of traditional nickel metallurgical waste for use as a valuable material that can be applied in the removal of organic amines from water systems. Silicon compounds from metallurgic waste were converted into dissolvable sodium silicate by roasting the waste with alkali. Silica with adsorption capacity was combined with magnetic NiFe cores by the carbonation decomposition of purified silicate solution. The composite magnetic adsorbent was characterized, and its adsorption mechanism for organic amines was investigated. The effects of the initial trimethylamine concentration, contact time and temperature on the adsorption efficiency of the composite adsorbent towards trimethylamine were investigated. It was found that the adsorption fit the Freundlich mode well. The adsorption kinetics can be described by a pseudo-second-order kinetic model. The adsorption capacity reached 55.8 μg/mg at 293 K. The use of metallurgical waste to prepare the magnetic composite adsorbent has three advantages, which include benefiting the environment by reducing the amount of solid waste and costs associated with constructing and maintaining storage facilities, generating valuable products in an economical manner and conveniently recycling used adsorbents to avoid secondary pollution.     

作为表面增强拉曼光谱基底的高度均匀Au纳米棒的构筑及对福美双的检测

采用种子生长法制备Au纳米棒(GNRs),随后进行组装和煅烧得到单层致密堆积的GNRs薄膜。在煅烧过程中,组装所需有机物在煅烧过程中分解,从而使得GNRs表面具有较高的清洁度。研究中发现,煅烧前后金纳米棒表面的间隙进一步提高,增强了其SERS(表面增强拉曼光谱)活性。为了研究其SERS活性,选择了2种探针分子以研究其灵敏度和均匀性,发现其具有较高的灵敏度和高的信号稳定性。随后将所制备的SERS基底成功用于检测超低浓度的农药分子。     

阿维菌素纳米水分散体的制备、表征及稳定性

利用阿维菌素具有2个活性羟基的特性,设计合成了一种具有阿维菌素结构单元的阴离子型聚氨酯分散剂,采用核磁共振和红外光谱表征了其结构.利用分散剂与阿维菌素结构的相似性,将溶有阿维菌素的分散剂溶液加入水中,制备了阿维菌素的纳米水分散体.研究分散剂中羧基含量及其分子量对分散体粒径的影响,结果表明,随着羧基含量的增加,分散体粒径逐渐降低,适当控制分子量有助于改善分散剂的分散能力.透射电镜显示分散粒子具有近似球形的形貌,粒径在20~40 nm之间.纳米分散体具有较高的离心稳定性和稀释稳定性.     

低温富集液液萃取-气相色谱-串联质谱法测定水样中15种农药残留

利用低温冷冻条件下农药在水相和有机相之间达到新的传质平衡,建立了低温富集液液萃取-气相色谱-三重四极杆串联质谱法同时测定水样中15种有机磷、有机氯及菊酯类农药的方法。通过对样品前处理中的溶剂选择、冷冻温度及冷冻时间的优化,最终确定的样品前处理条件为:萃取溶剂为甲苯2.0 mL;冷冻温度-40℃;冷冻时间1h。15种农药的检出限(3S/N)在0.005~0.02μg·L-1范围,测定下限(10S/N)为0.02~0.07μg·L-1。方法用于水样中农药的分析,加标回收率在78.8%~124%之间,测定值的相对标准偏差(n=5)在0.9%~9.1%之间。     

液相色谱串联质谱法测定水果中复硝酚钠残留量

以甲醇提取样品,采用超高效液相色谱串联质谱法(UPLC–MS/MS)测定水果中复硝酚钠的残留量。以甲醇–10 mmol/L乙酸铵水溶液(体积比为60∶40)为流动相,质谱采用电喷雾负离子MRM检测模式。对硝基苯酚钠和5-硝基愈创木酚钠的线性范围为0.05~2.00 mg/L,检出限为0.01 mg/kg,邻硝基苯酚钠的线性范围为2.5~100.0 mg/L,检出限为0.5 mg/kg,线性相关系数均大于0.995。实际样品中对硝基苯酚钠、邻硝基苯酚钠和5-硝基愈创木酚钠的加标回收率分别为83.0%~93.4%,81.0%~87.4%,83.0%~91.8%,测定结果的相对标准偏差小于7%(n=6)。该法操作简单、快捷,精密度、准确度高,适用于水果中复硝酚钠的残留分析。