Extraction and clean-up methods for organochlorine pesticides determination in milk

Organochlorine pesticides (OCPs) can cause environmental damage and human health risks since they are lipophilic compounds with high resistance to degradation and long half-lives in humans. As most persistent OCPs have been banned years ago, it is expected to find these compounds at trace levels in environment. Therefore, increasingly sensitive and reliable analytical techniques are required to ensure effective monitoring of these compounds. The aim of this review is to discuss extraction and clean-up methods used to monitor OCP residues in milk, reported in the last 20 years. To carry out this review, an exhaustive bibliographic review was conducted. Despite the disadvantages of conventional extraction and clean-up methods, such as liquid–liquid, solid-phase or Soxhlet extractions, these procedures are still used due to their reliability. New extraction methods, like solid-phase microextraction, matrix solid-phase dispersion or QuEChERS, have not been thoroughly evaluated for OCP determination in milk. Almost all the methodologies analyzed in this review presented good performance characteristics according to the performance acceptability criteria set in SANCO’s procedure. Comparison between limits of quantification (LOQ) and detection (LOD), for the reported methodologies, is not always possible due to the heterogeneity of the units. Thus, researchers should take into account an homogenization of LOD and LOQ units, according to the international regulations and MRLs established. Finally, more research is necessary to obtain the ideal methodology for OCPs determination in milk, which comprises the environmentally friendly characteristics of the new techniques and the reliability of the traditional methodologies.     

Evaluation of C18 solid‐phase extraction cartridges for the isolation of select pesticides and metabolites

Abstract

Nine different C₁₈ solid‐phase extraction (SPE) cartridges were evaluated for their efficiency at extracting nine pesticides and two s‐triazine metabolites from spiked deionized water samples. The SPE cartridges were found to contain nitrogen (N) and/or phosphorus (P) contaminants and varied in their extraction efficiency for certain pesticides and metabolites. Four of the nine SPE cartridges gave acceptable (70 to 120%) pesticide and metabolite recovery percentages, while five cartridges had marginal (50 to 70%) to poor (< 50%) recoveries. Statistical analyses showed that the poor to marginal recoveries found for three compounds could not be explained by considering several indigenous chemical and physical traits of the cartridge. It is suggested that proper SPE cartridge selection for pesticide recovery should be evaluated using several different cartridges.     

Restricted adaptive cluster sampling

Adaptive cluster sampling can be a useful design for sampling rare and patchy populations. With this design the initial sample size is fixed but the size of the final sample (and total sampling effort) cannot be predicted prior to sampling. For some populations the final sample size can be quite variable depending on the level of patchiness. Restricted adaptive cluster sampling is a proposed modification where a limit is placed on the sample size prior to sampling and quadrats are selected sequentially for the initial sample size. As a result there is less variation in the final sample size and the total sampling effort can be predicted with some certainty, which is impor- tant for many ecological studies. Estimates of density are biased with the restricted design but under some circumstances the bias can be estimated well by bootstrapping. © Rapid Science 1998     

Identifying the largest individual sample value from a two-way composite sampling design

Composite sampling techniques for identifying the largest individual sample value seem to be cost effective when the composite samples are internally homogeneous. However, since it is not always possible to form homogeneous composite samples, these methods can lead to higher costs than expected. In this paper we propose a two-way composite sampling design as a way to improve on the cost effectiveness of the methods available to identify the largest individual sample value.     

浊点萃取分离富集荧光光度法测定水中α - 萘酚

基于非离子表面活性剂Triton X-114,采用浊点萃取分离富集荧光光度法测定水中α-萘酚,优化了影响浊点萃取的各种因素,包括样品酸度、表面活性剂体积分数、氢氧化钠溶液浓度、平衡温度和时间等,讨论了常见无机离子和可能共存的有机物的干扰。方法在0.010 mg/L～0.400 mg/L范围内线性良好,检出限为3.0μg/L,标准溶液测定的RSD为4.8%,水样加标回收率为94.3%～103%。     

固相萃取- GC/MS法测定水中邻苯二甲酸酯类

采用固相萃取-GC／MS法测定水中6种邻苯二甲酸酯类有机污染物,比较了不同固相萃取柱对萃取效果的影响,优化了水样pH值、水样流量、穿透体积、洗脱溶剂、洗脱剂体积、洗脱流量等萃取条件。方法在0．050μg/L-800μg/L范围内线性良好,检出限为0．008μg/L～0．03μg／L,标准溶液测定的RSD≤10．5％,实际水样加标回收率为80．0％-100％。     

Extraction of labile metals from solid media by dilute hydrochloric acid

Extraction of labile metals from solid media is environmentally more meaningful than a total digestion. A variety of reagents have been introduced in the literature, but dilute HCl has received the greatest attention. We compare metal concentrations liberated by a dilute HCl leach with the sum of the 3-step optimized (standardized) BCR sequential extraction procedure. This is the first study to compare these procedures over a range of grain sizes. Road-deposited sediments from 10 sites in Honolulu were fractionated into six grain size classes. Aliquots of individual fractions were digested with dilute HCl, the 3-step BCR procedure (‘labile’), and a 4-acid (total) procedure. Results indicated that the weighted labile concentrations of Al, Cu, Fe, Mn, Ni, Pb and Zn were statistically greater than those from the dilute HCl leach. However, regression analysis indicated strong statistically significant relationships between the two partial extraction procedures for all metals. On a whole-sample basis, the toxicity classifications for anthropogenic-enhanced metals (Cu, Pb and Zn) were similar between extractions. Taken together, results suggest that the application of dilute HCl to solid media provides a rapid, cost-effective, and environmentally meaningful approach for contaminant monitoring.     

基于GB/T 29309标准的HALT测试技术分析

本文以标准GB/T 29309-2012为基础,以某款开关电源为例,对HALT试验设备、工作极限与破坏极限、试验步骤及设备运行中注意点等方面展开介绍,为电子产品可靠性测试提供相关探讨。     

海上平台采油工艺设计浅析

文章通过实例,简要阐述了滩海、浅海、深海三种开发模式的特点、主要工艺及其适用性。指出各自存在的问题,并提出相应的建议,为海上勘探开发提供借鉴。     

Indian dye yielding plants: Efforts and opportunities

The present review article deals with the information on the dye‐yielding plants of India. Dyes are intensively coloured compounds that are applied to a substrate such as fibre, paper, cosmetics, hair, etc. to give colours and can be extracted from the roots, fruits/berries, bark, leaves, flowers, and stem/wood, fungi, and lichens by various processes of extractions. In addition to their dye‐yielding characteristics, many of these plants possess medicinal values and can be used for multiple other purposes. Plant derived‐colours have an important role in human life because of their safe and eco‐friendly nature. But due to the availability of economically cheaper synthetic dyes, the indigenous knowledge of extraction, processing, and proper utilisation has been diminished. Nowadays, the demand for natural dyes has been increased worldwide due to awareness about their beneficial properties. It has been essential that proper documentation and measure of conservation should be undertaken to preserve these natural dye‐yielding plants. This review article is an aid to a collective inquiry into Indian dye plants.