Identification of microcystins from three collection strains of Microcystis aeruginosa

Microcystins (MCs) are toxic cyclic heptapeptides produced by various cyanobacteria genera, especially Microcystis. We identified 10 out of 12 MCs produced by three Microcystis aeruginosa strains from cyanobacteria collections, UTEX 2666, UTEX 2670 and UAM 1303, by using two analytical methods: Matrix-assisted Laser Desorption Ionization Time of Flight Mass Spectrometry (MALDI-TOF/MS) and HPLC Photodiode Array Detector coupled to a hybrid Quadrupole Time of Flight Mass Spectrometry (HPLC-PDA-QTOF/MS). MALDI-TOF/MS failed to detect non-polar MCs, such as MC-LY and MC-LW. HPLC-QTOF/MS permitted the accurate identification of most MCs present in methanolic extracts. Besides, three new MCs, namely: [D-Glu(OCH₃)⁶, D-Asp³] MC-LAba, MC-YL and MC-YM were detected by HPLC-QTOF/MS.     

Rapid detection of toxic metals in non-crushed oyster shells by portable X-ray fluorescence spectrometry

The aim of this study was the multi-elemental detection of toxic metals such as lead (Pb) in non-crushed oyster shells by using a portable X-ray fluorescence (XRF) spectrometer. A rapid, simultaneous multi-element analytical methodology for non-crushed oyster shells has been developed using a portable XRF which provides a quick, quantitative, non-destructive, and cost-effective mean for assessment of oyster shell contamination from Pb. Pb contamination in oyster shells was further confirmed by scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS). The results indicated that Pb is distributed in-homogeneously in contaminated shells. Oyster shells have a lamellar structure that could contribute to the high accumulation of Pb on oyster shells.     

超声波提取-GC/MS法测定生物体内硝基苯类化合物

以洪泽湖中6种代表性生物为研究对象，采用超声波法提取样品中硝基苯类化合物，用凝胶色谱净化、浓缩，气相色谱／质谱联用法测定。该法与索氏提取法在同等试验条件下进行加标回收试验，前者回收率高且稳定，简便可行。方法检出限为0．008μg／g～0．030μg／g，平均加标回收率为76．5％～109％，重复测定3次的RSD为1．5％～13．0％。     

Lindane removal by pure and mixed cultures of immobilized actinobacteria

Stereoselective dissipation of epoxiconazole had been studied in grape and soil during plant growing under field conditions in this paper. A sensitive and rapid chiral method was developed and validated for the determination of epoxiconazole stereoisomers in grape and soil based on liquid chromatography coupled with triple quadrupole mass spectrometry (LC-MS/MS). Phenomenex Lux Cellulose-1 column was used for enantioseparation with a mixture of acetonitrile/water (90/10, v/v) as mobile phase at flow rate of 0.3 mL min⁻¹. Fortified recoveries in grape and soil samples ranged from 76.0% to 91.9% and relative standard deviations were less than 11.4% with fortified levels of 0.025-1.0 mg kg⁻¹. The limits of detection and quantification were 0.005 mg kg⁻¹ and 0.025 mg kg⁻¹, respectively, with linear calibration curves extending up to 5.0 mg kg⁻¹. The field experimental results showed that dissipations of epoxiconazole stereoisomers in grape followed first-order kinetics (R² > 0.92) and stereoselectivity occurred in 2 h after spraying. The (−)-stereoisomer with half-life of 9.3 d degraded faster than (+)-stereoisomer with that of 13.2 d, and resulted in relative enrichment of (+)-stereoisomer. However, the stereoisomeric dissipations in soil were triphasic (“increase-decrease-steady”) with lower dissipation rates, and also occurred with preferential degradation of (−)-stereoisomer under field condition. The results for stereoselective dissipations can be applied for food and environmental assessments of chiral pesticides.     

A new direct thermal desorption-GC/MS method: Organic speciation of ambient particulate matter collected in Golden, BC

Particulate matter having an aerodynamic diameter less than 2.5 μm (PM2.5) is thought to be implicated in a number of medical conditions, including cancer, rheumatoid arthritis, heart attack, and aging. However, very little chemical speciation data is available for the organic fraction of ambient aerosols. A new direct thermal desorption-gas chromatography/mass spectrometry (TD-GC/MS) method was developed for the analysis of the organic fraction of PM2.5. Samples were collected in Golden, British Columbia, over a 15-month period. n-Alkanes constituted 33–98% by mass of the organic compounds identified. PAHs accounted for 1–65% and biomarkers (hopanes and steranes) 1–8% of the organic mass. Annual mean concentrations were: n-alkanes (0.07–1.55 ng m⁻³), 16 PAHs (0.02–1.83 ng m⁻³), and biomarkers (0.02–0.18 ng m⁻³). Daily levels of these organics were 4.89–74.38 ng m⁻³, 0.27–100.24 ng m⁻³, 0.14–4.39 ng m⁻³, respectively. Ratios of organic carbon to elemental carbon (OC/EC) and trends over time were similar to those observed for PM2.5. There was no clear seasonal variation in the distribution of petroleum biomarkers, but elevated levels of other organic species were observed during the winter. Strong correlations between PAHs and EC, and between petroleum biomarkers and EC, suggest a common emission source – most likely motor vehicles and space heating.     

Headspace-SPME-GC-MS Identification of Volatile Organic Compounds Released from Expanded Polystyrene

A method for the identification of volatile organic compounds (VOCs) released from packaging expanded polystyrene (EPS) is presented. Headspace solid-phase microextraction (HS-SPME) with a 75-m carboxen-polydimethylsiloxan fiber was used as sample preparation technique before the determination of the volatile organic compounds by gas chromatography–mass spectrometry (GC-MS). For separation of compounds, two fused silica capillary columns of different polarity (DB-5ms and BPX-50) were used. Styrene monomer with his impurities and oxidation products, as well as residual pentane, were identified in the headspace of EPS.     

Reusability of sewage sludge in clay bricks

Bricks produced from sewage sludge in different compositions were investigated. Results of the tests indicated that the sludge proportion is a key factor in determining the brick quality. Increasing the sludge content results in a decrease in brick shrinkage, bulk density, and compressive strength. Brick weight loss on ignition was mainly due to the contribution of the contained organic matter from the sludge being burnt off during the firing process, as well as inorganic substances found in both clay and sludge. The physical, mechanical, and chemical properties of the bricks that were supplemented with various proportions of dried sludge from 10 to 40wt% and generally complied with the General Specification for Brick as per the Malaysian Standard MS 7.6:1972, which dictates the requirements for clay bricks used in walling in general. A standard leaching test method also showed that the leaching of metals from the bricks is very low.     

海水中有机污染物的气相色谱－质谱法鉴定

本文采用一种简便的连续萃取装置．对海水中痕量有机物进行富集，大量的海水被萃取后，萃取物经干燥浓缩在毛细管气相色谱上进行了分离，并用质谱－计算机自动检索装置进行了定性鉴定，共确定出３６种组分。本方法的检测限为辛烷１０ｐｐｔ。     

GC/MS法测定润滑油基础油中多环芳烃

对润滑油基础油中多环芳烃的气相色谱/质谱(GC/MS)测定方法进行了研究,探讨了样品的提取,固相萃取柱净化等前处理方法,同时也对仪器测定条件进行了优化.结果表明,在检测润滑油基础油中多环芳烃时,经优化的GC/MS法的加标回收率和精密度均达到较满意的水平.     

G C/MS法测定环境空气中痕量POPs类有机氯农药及降解产物

采用快速溶剂萃取-氟罗里硅土柱净化-气相色谱/质谱联用法测定环境空气中POPs类有机氯农药及其降解产物.艾氏剂、狄氏剂、异狄氏剂、六六六、滴滴涕,七氯、氯丹、灭蚁灵及其降解产物的检出限为2.0 ng～4.6 ng,空白加标回收率为62.1%～118%,RSD为6.8%～15.2%.