6种有机磷农药标准溶液不确定度分析

分析了乙酰甲胺磷、乙硫磷、丙线磷、苯硫磷、特丁磷、硫线磷6种有机磷农药标准溶液研制过程中测量不确定度的影响因素,并计算出有机磷标准溶液质量浓度的扩展不确定度.不确定度分量中,配制过程和溶液稳定性的不确定度是主要的.     

啤酒中有机氯及拟除虫菊酯残留检测方法研究

建立同时检测啤酒中17种有机氯及拟除虫菊酯农药残留的气相色谱检测方法,样品经过正己烷提取,采用弗罗里硅土柱净化,GC-ECD法同时检测,外标法定量,方法回收率为80.1%～115.5%,RSD为2.10%～6.95%,方法检测限为：0.0003～0.0031 mg/kg。     

氨汽提法尿素装置中压甲铵冷凝器防结垢工艺优化

针对氨汽提法尿素装置中压甲铵冷凝器管侧冷却水结垢的问题,对2套解决方案进行了比较,选用蒸汽冷凝液密闭循环冷却方案对循环冷却水系统进行了工艺优化设计.     

Assessment of safety margins of exposure to non-genotoxic chemical substances in food

The concept of Food Safety Margin (FSM) was introduced in microbiological risk analysis as an alternative approach to risk characterization within the informed-risk decision-making process. Its aim was to verify compliance with food safety objectives by assessing the effects of uncertainties. This paper describes the fundamentals and develop a new formulation of safety margins to verify compliance with food safety goals in relation to exposure to non-genotoxic chemical hazards. Both classical and probabilistic metrics were used to compare a given exposure to an estimated daily intake (EDI) with a given safety goal, the acceptable daily intake (ADI). The safety margins of these metrics were assessed in the exposure of peaches to organophosphorus pesticides. The pesticides considered were Azinphos-methyl, Chlorpyrifos, Diazinon, Dimethoate, Methamidophos, Parathion-methyl and Phosmet. The concentrations were obtained from the USDA pesticide database. The study period included the 11 years in which peaches were analysed from 1994 to 2014. The results show the importance of using the effect of uncertainty instead of mean values for risk characterization and that not only safety margins increased during this period but also that uncertainty was reduced. In general, large safety margins were observed in the period studied and few situations were found in which exposure was outside the safety limits.     

A survey of levels of ethyl carbamate in alcoholic beverages in 2009–2012, Hebei Province,China

Results of a survey of levels of ethyl carbamate (EC) (urethane) in alcoholic beverages carried out in four successive years from 2009 to 2012 by gas chromatography-mass spectrometry (GC/MS) are presented. The beverages were purchased for sampling from Hebei Province of China, including eight main areas of production. The samples comprised wines (n = 212), grain spirits (n = 143) and wine sauces (n = 164). The data show that the average EC content in these kinds of alcoholic beverages remains nearly constant over the years. The results provide valuable data for food authorities to establish maximum limits for EC in China.     

Assessment of PCDD/F,PCB, OCP and BPA dietary exposure of non-breast-fed European infants

The aim of this study is to obtain data on the exposure of non-breast-fed infants to polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/F), polychlorinated biphenyls (PCB), organochlorine pesticides (OCP), and bisphenol A (BPA) and its chlorinated derivatives through consumption of commercial infant foods with largest shares of the market in 22 European Union countries. The E-Screen bioassay was employed to assess the oestrogenicity of the baby foods and the ethoxyresorufin-O-deethylase (EROD) induction was measured to determine the levels of PCDD/F and PCB. Consequently, the highest total effective xenoestrogen burden (TEXB) of 73.60?pM?Eeq?g^?1 was found in the soy-based formula and the EROD bioassay was always below the limit of quantification (LOQ) (3.5?pg?g^?1). Overall, the estimated dietary exposure to BPA via commercial baby foods was lower than the tolerable daily intake (TDI) of 50?µg?kg^?1 body weight (bw). Furthermore, the findings indicated that the dietary exposure of 0–9-month-old infants through the products investigated here does not exceed the maximum TDI of 4?pg WHO-TEQ (toxic equivalents)?kg^?1 bw. However, exposure to more than 2?pg WHO-TEQ?kg^?1?bw?day^?1 might occur for 0–4-month-old infants consuming ‘starting’ hypoallergenic formula. Moreover, analysis of OCP indicated that the dietary exposure of non-breast-fed infants was not harmful. Considering the importance of early development and the vulnerability of infants and children, it is essential to determine their dietary exposure to contaminants in order to decide which efforts of risk reduction should receive highest priority.     

Multi-residue method for the analysis of pesticides in Arabica coffee using liquid chromatography/tandem mass spectrometry

Coffee is a major tropical agricultural commodity and represents a significant fraction of the economy of many countries. However, certain plant and animal species can damage coffee crops, affecting trade. A solution to this issue is the use of pesticides, some of which are harmful to human health and the environment. This work consisted of the development of a multi-residue method for the analysis of pesticides in coffee by using LC-MS/MS. The QuEChERS extraction procedure was used. The following analytical parameters were optimised: selectivity, analytical range, linearity, LOD, LOQ, precision (RSD%) and recovery of the method. The results showed that the method is selective, as they were linear in the range of 10.0–100.0 µg kg^?1. The sensitivity, recovery and precision were adequate for the multi-residue analysis of pesticides in coffee. The method was applied to the analyses of 15 Brazilian coffee samples.     

Solid-phase microextraction-liquid chromatography-mass spectrometry applied to the analysis of insecticides in honey

An approach based on solid-phase microextraction-liquid chromatography-mass spectrometry (SPME-LC-MS) has been developed for determining 12 insecticides (bromophos ethyl, chlorpyrifos methyl, chlorpyrifos ethyl, diazinon, fenoxycarb, fonofos, phenthoate, phosalone, pirimiphos methyl, profenofos, pyrazophos, and temephos) in honey. The influence of several parameters on the efficiency of the SPME was systematically investigated. Under optimal conditions, the procedure provided excellent linearity (>0.990), detection and quantification limits (between 0.001 and 0.1?µg?g^?1 and between 0.005 and 0.5?µg?g^?1, respectively), and precision (<19% at the quantification limits and from 6 to 14% at ten times higher concentrations). However, recoveries were not so good, ranging from 19 to 92%. Honey samples were found that were contaminated with bromophos ethyl, diazinon, fonofos, pirimiphos ethyl, pyrazophos, and temephos at estimated concentrations from 6.2?±?1.2 to 19?±?3?ng?g^?1.     

Combination of supercritical fluid extraction with dispersive liquid-liquid microextraction for extraction of organophosphorus pesticides from soil and marine sediment samples

Supercritical fluid extraction (SFE) coupled with dispersive liquid-liquid microextraction (DLLME) and followed by gas chromatography-flame ionization detection (GC-FID) was applied for extraction and determination of ultra-trace amounts of seven organophosphorus pesticides (OPPs) (o,o,o-triethyl phosphorothioate, thionazin, sulfotepp, disulfoton, methyl parathion, parathion, and famphur) in soil and marine sediment samples. Supercritical CO₂ at 150 bar, 60 °C, 10 min static and 30 min dynamic extraction times was used to extract the pesticides. The extracts were collected in 1.0 mL of acetonitrile. Seventeen μL of carbon tetrachloride was dissolved in the collecting solvent and the mixture was then injected rapidly into 5.0 mL of aqueous solution. About (5.0 ± 0.2 μL) of sediment phase was collected after centrifuging and finally 2.0 μL of it was injected into gas chromatography (GC) injection port for analyses. The extraction recoveries for the target analytes were in the range of 44.4% and 95.4% and relative standard deviation (RSD%) for four-replicate measurements was below 7.5%. The limit detections of the method for determining the pesticides were in the range of 0.001-0.009 mg kg⁻¹. The method was successfully applied for analysis of OPPs in real soil and marine sediment samples and satisfactory results were obtained.     

An efficient extraction and clean‐up procedure for pesticide determination in olive oil

This work reports a simple, rapid, and effective extraction method based on liquid–liquid extraction (LLE) followed by matrix solid‐phase dispersion‐sonication for detection, identification and quantification of multiclass pesticides in virgin olive oil using liquid chromatography mass spectrometry (LC‐QTOF‐MS). LLE to extract pesticide residues in virgin olive oil was performed in order to study the centrifugation efficiency to obtain high recovery yield and low co‐extract fat residue in the final extract. Different suitable parameters of MSPD procedure were evaluated, such as nature of dispersing phase, clean‐up adsorbent, and volume of eluting solvent (acetonitrile) in different extraction conditions, with or without sonication. The best results were obtained using 5 g of virgin olive oil, 2 g of PSA as dispersant sorbent, 2 g of Florisil/GCB (70:30 w/w) as clean‐up sorbent, and 15 mL of acetonitrile as eluting solvent under conditions of 15 min ultrasonic bath at RT. Method validation was performed in order to study sensitivity, linearity, precision, and accuracy. Average recoveries ranged between 73.7 and 104.2% with relative SDs 5.3–13.4% at three concentration levels (25, 50, and 100 µg/kg). Detection and quantification limits ranged from 1.5 to 5 µg/kg and 3 to 9 µg/kg, respectively.