Evaluation of a screening method for classifying virgin and recycled paper and board samples

This paper deals with the study of volatile compounds released by recycled paper and board. The aim of the study was to demonstrate the feasibility of headspace procedure coupled to gas chromatography/mass spectrometry (GC/MS) applied to complex paper‐based samples together with a chemometric procedure as a powerful method for screening potential volatile contaminants released by the recycled and virgin paper samples. Using this procedure, the identification of virgin or recycled paper could be achieved based on the identification on specific markers of the recycled pulp. Fifteen different samples within virgin and recycled paper were studied. After equilibration, the vapour phase of the samples was analysed by automatic headspace coupled online to GC/MS. The analytical approach for volatile compounds, their identification and the selection of some compounds as markers for recycled pulp are shown and discussed. A discriminate analysis applied to the set of results obtained allows classification of the samples into four different groups according to the content of recycled pulp (0, 10–30 and > 80% of recycled pulp), the surface treatment of the paper (no surface treatment, clay coating and plastic coating), the grammage (from < 100 to > 300 g/m²) and the sample thickness (from < 300 to > 600 µm). The matrix effect on the volatilization of some compounds from the paper samples and the analytical behaviour are also discussed. Copyright © 2009 John Wiley & Sons, Ltd.     

Effect of cooking or handling conditions on the furan levels of processed foods

The aim of this study was to investigate the possible effects of cooking or handling conditions on the concentration of furan in processed foods. The analytical method used to analyse furan levels in foods was optimized based on solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS). In baby soups, the concentration of furan decreased by up to 22% after opening a lid for 10 min. In the baby food in retort packaging, the level of furan was reduced by 15–33% after heating the foods at 50°C without a lid. Furan in rice seasonings was evaporated completely after heating the foods at 60°C. Regarding powered milk, the levels of furan were too low to be compared under various conditions. The levels of furan decreased to 58% in beverage products for babies, after storing them at 4°C for 1 day without a lid. The levels of furan in canned foods such as cereal and vegetable were reduced by zero to 52% when they were stored without stirring in a refrigerator at 4°C for 1 day. When we boiled canned fish, the furan present was almost completely evaporated. It is recommended that canned meats be heated up to 50–70°C for the reduction (26–46%) of furan levels. The levels of furan in instant and brewed coffee samples were significantly reduced after storing for 11 to 20 min at room temperature without a lid (p < 0.05).     

Determination of 15 β-lactam antibiotics in pork muscle by matrix solid-phase dispersion extraction (MSPD) and ultra-high pressure liquid chromatography tandem mass spectrometry

An UPLC–MS/MS method based on matrix solid-phase dispersion (MSPD) was developed for simultaneous determination of 15 β-lactams in pork muscle. Muscle tissue was blended with Oasis HLB adsorbent. A column made from the sorbent/muscle tissue matrix was washed with hexane, after which β-lactams was eluted with acetonitrile/water (50:50, v/v) both containing 0.1% formic acid. The final extract was evaporated, and reconstituted into acetonitrile/water (10:90, v/v) for the analysis of UPLC-MS/MS. The correlation coefficient (r²) with each matrix-matched calibration curve is higher than 0.99. Limits of detection (LODs) and limits of quantification (LOQs) of β-lactams were ranged from 0.02 to 0.63 μg kg⁻¹ and 0.07–0.97 μg kg⁻¹, respectively. At the fortified levels, mean recoveries of all compounds were ranged from 92 to 111%, and the RSDs were lower than 12%. The method was accurate and reproducible, being successfully applied to the monitoring of 15 β-lactams in pork muscles obtained from the Chinese market.     

Characterization of Volatile Compounds in Microfiltered Pasteurized Milk Using Solid-Phase Microextraction and GC×GC-TOFMS

Volatiles of milk were characterized by solid-phase microextraction coupled with comprehensive two-dimensional gas chromatography and time-of-flight mass spectrometry. Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry two-dimensional gas chromatography with time-of-flight mass spectrometry not only separated the 52 compounds that co-elute in conventional gas chromatography-mass spectrometry, but also identified 107 compounds that were first reported in milk. These volatiles included aliphatic hydrocarbons (69), aromatic hydrocarbons (42), ketones (28), esters (16), aldehydes (14), alcohols (14), acids (14), nitrogenous compounds (9), ethers (8), and sulfo compounds (3). Five dominant volatiles were hexanoic acid (193.57 ng/mL milk), methoxy-phenyl-oxime (114.83 ng/mL milk), octanoic acid (109.38 ng/mL milk), 4,5-dimethyl-1-hexene (101.48 ng/mL milk), and 2-Pentanone (99.74 ng/mL milk). This proposes an improvement methodology for determining the volatiles of dairy products.     

Solid-phase extraction for simultaneous separation and preconcentration of Fe(III) and Zn(II) traces using three chelatants and Ramelak bark-derived activated carbon as a new bio-sorbent

This article introduces a comparative study for the simultaneous separation and preconcentration of Fe(III) and Zn(II) traces in various water samples using three well-known ligands as chelating agents and activated carbon (AC) derived from Ramelak bark as a new bio-sorbent prior to the determination by ?ame atomic absorption spectrometry. The chelating agents were 4,4’-[(4-Cyano-phenyl)methylene]bis(3-methyl-1-phenyl-1H-pyrazol-5-ol) (CMBM), diethyldithiocarbamate (DDTC) and ammonium pyrrolidine dithiocarbamate (APDC). CMBM was synthesized by a procedure reported in the literature. The newly prepared AC was characterized by Scanning Electron Microscopy (SEM) and Fourier-Transform Infrared (FTIR) Spectrometry. The analytical parameters affecting the separation efficiency of the analytes including pH, shaking time, chelating agent volume (concentration), sorbent mass, sample ?ow rate and elution conditions were investigated and discussed. Common coexisting ions did not seriously interfere with the separation, showing the good selectivity of the proposed method. The calibration graph was linear in the range of 0.35–70, 0.50–80, 0.9–100, 0.55–75, 0.75–90 and 1.0–120 ng mL^?1 for Fe-CMBM, Fe-DDTC, Fe-APDC, Zn-CMBM, Zn-DDTC and Zn-APDC, respectively. Under optimized conditions, the limits of detection were 0.11, 0.13, 0.27, 0.16, 0.22 and 0.30 ng mL^?1 for Fe-CMBM, Fe-DDTC, Fe-APDC, Zn-CMBM, Zn-DDTC and Zn-APDC, respectively. The proposed method has been applied to the determination of Fe(III) and Zn(II) in different water samples with satisfactory recovery percentages. The developed method, validated with standard reference materials, was used successfully in determining the concentrations of metal ions in water samples.     

固相微萃取联用气相色谱测定有机磷农药

以溶胶-凝胶方法制备的聚甲基苯基乙烯基硅氧烷／羟基硅油复合涂层的固相微萃取探头（PMPVS／OH-TSO）联用气相色谱测定了有机磷农药。同时对固相微萃取的最佳奈件进行了优化，该探头较商用探头有更高的萃取能力。方法的检测限分别为2．1μg／L（敌敌畏）、1．5μg／L（甲基对硫磷），相对标准偏差均不大于7．4％，线性范围均为2个数量级。对某灌溉水中残留的有机磷农药进行了测定，但以上的OPPs均没有检测到，其回收率分别为83．6％和93．4%。     

Components detected by means of solid-phase microextraction and gas chromatography/mass spectrometry in the headspace of artisan fresh goat cheese smoked by traditional methods

The study of the headspace components of fresh smoked goat cheese, was carried out by means of solid-phase microextraction using a polyacrylate fiber followed by gas chromatography/mass spectrometry. The samples studied were six artisan Palmero cheeses manufactured following traditional methods and smoked using pine needles. The cheese regions studied were exterior, interior, and a cross section. In total, more than 320 components were detected, the exterior region being the richest in components, among which were acids, alcohols, esters, hydrocarbons, aldehydes, ketones, furan and pyran derivatives, terpenes and sesquiterpenes, nitrogen derivatives, phenol, guaiacol and syringol derivatives, ethers, and others. In addition to typical cheese components, typical smoke components were also detected; these latter were present especially in the headspace of the exterior region and only those in significant concentrations in the exterior region were also detected in the interior. The main components were acids and phenolic derivatives. These latter compounds play an important role in the flavor of this cheese, and their relative proportions together with the presence of specific smoke components derived from pine leaves may be considered of interest in order to distinguish this cheese from others smoked with different vegetable matter.     

水中OCPs预处理方法比较

采用GC/μECD作为检测手段,比较了三种预处理方法:液液萃取、固相萃取、固相微萃取对水中OCPs的线性关系和回收情况.三种方法中,固相微萃取定量曲线的相关系数在0.9499至0.9996之间,且总体水平相对较低;液液萃取和固相萃取的相关系数在0.9948至0.9993之间.与液液萃取相比,固相萃取的回收效果更好,并且减少了人工和溶剂的消耗.采用固相萃取多次分析自来水中17种OCPs的残留水平,检出10种物质,所得浓度均未超过国内外相关水质标准.