Homogeneous liquid-liquid extraction combined with gas chromatography-electron capture detector for the determination of three pesticide residues in soils

In this study, a new method was developed for analyzing malathion, cypermethrin and lambda-cyhalothrin from soil samples by using homogeneous liquid–liquid extraction (HLLE) and gas chromatography with electron capture detector (GC–ECD). Acetone was used as extraction solvent for the extraction of target pesticides from soil samples. When the extraction process was finished, the target analytes in the extraction solvent were rapidly transferred from the acetone extract to carbon tetrachloride, using HLLE. Under the optimum conditions, linearity was obtained in the range of 0.05–40 μg kg⁻¹ for malathion, 0.04–10 μg kg⁻¹ for lambda-cyhalothrin and 0.05–50 μg kg⁻¹ for cypermethrin, respectively. Coefficients of correlation (r²) ranged from 0.9993 to 0.9998. The repeatability was carried out by spiking soil samples at concentration levels of 2.5 μg kg⁻¹ for lambda-cyhalothrin, and 10 μg kg⁻¹ for malathion and cypermethrin, respectively. The relative standard deviations (RSDs) varied between 2.3 and 9.6% (n = 3). The limits of detection (LODs), based on signal-to-noise ratio (S/N) of 3, varied between 0.01 and 0.04 μg kg⁻¹. The relative recoveries of three pesticides from soil A1, A2 and A3 at spiking levels of 2.5, 5 and 10 μg kg⁻¹ were in the range of 82.20–91.60%, 88.90–110.5% and 77.10–98.50%, respectively. In conclusion, the proposed method can be successfully applied for the determination of target pesticide residues in real soil samples.     

N2双流体细水雾抑制管道瓦斯爆炸实验研究

为了在较低压力下获得较小粒径的细水雾,降低喷雾抑爆系统的运行成本,提高系统的适用性和抑爆效率,自行搭建了尺寸为120 mm×120 mm×840 mm的透明有机玻璃瓦斯爆炸管道实验平台。采用双流体喷嘴将N₂和细水雾送入试验管道,通过调节喷雾压力和喷雾时间开展了双流体细水雾抑制瓦斯爆炸实验研究,从火焰速度、瓦斯爆炸超压2个方面探讨双流体细水雾的抑爆有效性。实验结果表明:N₂双流体细水雾抑爆效果明显,可以减小瓦斯爆炸强度;随着喷雾时间的延长,爆炸火焰的速度峰值逐渐下降,爆炸超压峰值逐渐下降,平均升压速率逐渐降低;当N₂压力为0.4 MPa、喷雾时间为3 s时,速度峰值比不喷雾时下降60.39%,爆炸超压峰值下降37.76%。     

Analysis of PAHs in Water and Fruit Juice Samples by DLLME Combined with LC-Fluorescence Detection

A simple, rapid and efficient method termed dispersive liquid–liquid microextraction combined with liquid chromatography-fluorescence detection, has been developed for the extraction and determination of polycyclic aromatic hydrocarbons (PAHs) in water and fruit juice samples. Parameters such as the kind and volume of extraction solvent and dispersive solvent, extraction time and salt effect were optimized. Under optimum conditions, the enrichment factors ranged from 296 to 462. The linear range was 0.01–100 μg L^?1 and limits of detection were 0.001–0.01 μg L^?1. The relative standard deviations (RSDs, for 5 μg L^?1 of PAHs) varied from 1.0 to 11.5% (n = 3). The relative recoveries of PAHs from tap, river, well and sea water samples at spiking level of 5 μg L^?1 were 82.6–117.1, 74.9–113.9, 77.0–122.4 and 86.1–119.3%, respectively. The relative recoveries of PAHs from grape and apple juice samples at spiking levels of 2.5 and 5 μg L^?1 were 80.8–114.7 and 88.9–123.0%, respectively. It is concluded that the proposed method can be successfully applied for determination of PAHs in water and fruit juice samples.     

湿法炼锌净化液中痕量锗的在线分析

本文采用非间隔流动分析技术，建立了一种在线测定硫酸锌溶液中痕量锗的方法。显色体系为ＨＣｌ－水杨基荧光酮－乳化剂ＯＰ，并用多波长光度法克服了试样中高浓度硫酸锌以及背景吸收的影响，采样频率３０样／ｈ，测定范围１０－１００μｇ／Ｌ。该方法已用于锌冶冻厂净化过程中痕量锗的在线分析。     

一种自动微量滴定新方法

本文依据传统滴定分析原理，利用流动注射装置提出一种新的自动微量滴定方法，它不仅具有流动注射滴定分析法简便快速，试剂和试样消耗少，仪器装置简单等优点，而且测定信号怀被测组分的浓度直接成线性关系，结果的准确度和精度优于一般流动注射滴定方法。通过用盐酸滴定氢氧化钠进行验证，相关系数为０．９９９９，相对标准偏差（ＲＳＤ）为０．４％。     

短波近红外过程分析仪的研制与应用

本文介绍一种短波近红外(700～1100nm)过程分析仪的研制与应用。仪器在722型单光束光栅分光光度计的基础上研制成,包括光源、光栅单色器、硅探测器、信号放大、A/D转换、8位单片微型计算机、数码显示和RS-232C串行通讯接口等几部分,它具有光谱扫描、串行通讯及分析结果预测功能。仪器校正采用PLS(偏最小二乘)回归法。在应用方面,根据氨水在短波红外区的吸收光谱,利用所研制的仪器实现了氨浓度的非破坏性分析,对于氨浓度为0～13.5mol/L的试样,预测标准差(SEP)为0.116mol/L。     

Determination of Two Pesticides in Soils by Dispersive Liquid–Liquid Microextraction Combined with LC-Fluorescence Detection

In the present work, a simple, rapid and sensitive sample pre-treatment technique, dispersive liquid–liquid microextraction (DLLME) coupled with liquid chromatography-fluorescence detection (LC-FLD), has been developed to determine carbamate (carbaryl) and organophosphorus (triazophos) pesticide residues in soil samples. Methanol was first used as extraction solvent for the extraction of pesticides from the soil samples and then as dispersive solvent in the DLLME procedure. Under the optimum extraction conditions, the linearity was obtained in the concentration range of 0.1–1,000 ng g⁻¹ for carbaryl and 1–5,000 ng g⁻¹ for triazophos, respectively. Correlation coefficients varied from 0.9997 to 0.9999. The limits of detection (LODs), based on signal-to-noise ratio (S/N) of 3, ranged from 14 to 110 pg g⁻¹. The relative standard deviation (RSDs, for 20.0 ng g⁻¹ of each pesticide) varied from 1.96 to 4.24% (n = 6). The relative recoveries of two pesticides from soil A1, A2 and A3 at spiking levels of 10.0, 20.0 and 50.0 ng g⁻¹ were in the range of 88.2–108.8%, 80.8–110.7% and 81.0–111.1%, respectively. The results demonstrated that DLLME was a sensitive and accurate method to determine the target pesticides, at trace levels, in soils.

     

Hypocrellin B-mediated sonodynamic action induces apoptosis of hepatocellular carcinoma cells

Objective

The present study aims to investigate apoptosis of hepatocellular carcinoma cells induced by hypocrellin B-mediated sonodynamic action.

Methods

The hypocrellin B concentration was kept constant at 2.5 μM and cells from the hepatocellular carcinoma HepG2 cell line were exposed to ultrasound with an intensity of 0.46 W/cm² for 8 s. Cell cytotoxicity was quantified using an MTT assay 24 h after sonodynamic therapy (SDT) of hypocrellin B. Apoptosis was investigated using a flow cytometry with Annexin V-FITC and propidium iodine staining. Intracellular reactive oxygen species (ROS) levels were detected using a flow cytometry with 2,7-dichlorodihydrofluorecein diacetate (DCFH-DA) staining.

Results

The cytotoxicity of hypocrellin B-mediated sonodynamic action on HepG2 cells was significantly higher than those of other treatments including ultrasound alone, hypocrellin B alone and sham treatment. Flow cytometry showed that hypocrellin B-induced sonodynamic action markedly enhanced the apoptotic rate of HepG2 cells. Increased ROS was observed in HepG2 cells after being treated with hypocrellin B-mediated sonodynamic action.

Conclusions

Our data demonstrated that hypocrellin B-mediated sonodynamic action remarkably induced apoptosis of HepG2 cells, suggesting that apoptosis is an important mechanism of cell death induced by hypocrellin B-mediated SDT.