近岸海水中全氟化合物的液相色谱-离子阱质谱法测定

建立了利用高效液相色谱-电喷雾离子阱质谱(HPLC-ESI-IT-MS/MS)测定近岸海水中多种常见全氟化合物(PFCs)的分析方法.采用固相萃取法(SPE)对海水中的PFCs净化富集,用HPLC-ESI-IT-MS/MS多反应离子监测(MRM)模式对各组分(全氟己烷磺酸、全氟辛烷磺酸、全氟辛烷磺酰胺、全氟己酸、全氟庚酸、全氟辛酸、全氟壬酸、全氟癸酸、全氟十一酸、全氟十二酸)进行测定.在最佳实验条件下,采用基质匹配标准曲线法定量,以消除海水基质的影响,8种目标化合物的检出限介于0.50—1.00 ng·L-1,9种PFCs的回收率在71.0%—130.2%之间,能满足近岸海水中多种PFCs检测的要求.青岛沿岸表层海水样品测定结果显示,全部采样站点的海水样品中均检测到≥4种PFCs,说明青岛沿岸海水中已有一定程度的PFCs污染.     

微囊藻毒素-LR的提取与测定

采用固相萃取结合液相色谱的方法,对可能有微囊藻毒素污染的某水库中的藻体和水样分别进行提取分析,在藻体中检测出微囊藻毒素LR,并确定产毒的藻种为水华微囊藻。同时对微囊藻毒素LR的测定方法进行了一定探讨。     

常规液相色谱柱测定早熟素Ⅱ的方法探讨

通过使用市售的常规C18液相色谱柱(规格:150mm×4.6mm,5 μm),探讨了早熟素Ⅱ的分析方法并对其进行了可行性论证.以V(甲醇):V(水)=80:20为流动相,流量1 mL·min~(-1),检测波长为224nm,柱温35℃.得出早熟素Ⅱ在8～108μg·mL~(-1)的范围内呈良好的线性关系(相关系数,为0.99997),最低检出限为1.0379μg·mL~(-1)(信噪比为3),加标回收率为93.3%～104.98%,变异系数为0.12%～4.41%.与使用非常规色谱柱分析早熟索Ⅱ的方法相比,该方法采用了市售常规柱,能够更大限度地满足实验条件,通用性更强.     

上海市大气PM2.5中羰基化合物的研究

利用2,4-二硝基苯肼(DNPH)作为衍生化试剂,高效液相色谱/紫外检测法(HPLC/UV)定量检测上海市大气PM2.5中单羰基和二羰基化合物,共检测出5种单羰基化合物和2种二羰基化合物(乙二醛和甲基乙二醛).单羰基化合物中浓度最高的是甲醛和乙醛,其年平均浓度分别为(1579.47±672.81)ng/m3和(572.02±470.58)ng/m3;二羰基化合物乙二醛和甲基乙二醛的年平均浓度分别为(63.74±54.27)ng/m3和(97.28±39.62)ng/m3.研究发现上海市大气PM2.5中一些羰基化合物具有明显的日变化和季节变化规律:日变化表现为早晚高峰,而季节性变化单羰基化合物是冬天>夏天,二羰基化合物则是夏季>冬季.此外,PM2.5中羰基化合物的浓度还与温度、湿度、质量浓度具有一定的关系.     

High performance liquid chromatographic determination of pesticides in soluble phase and suspended phase in river water

A high performance liquid chromatographic method has been developed to determine pesticides in river water as both dissolved phase and suspended phase. The target pesticides were eight herbicides, asulam, diuron, flazasulfuron, linuron, MCPB, mecoprop, pyrazosulfuron‐ethyl and siduron, and two fungicides, oxine‐copper and thiram. The pesticides in filtered river water were extracted with styrene‐divinylbenzene copolymer and were eluted with acetonitrile. The pesticides on suspended solids were extracted ultrasonically with acetonitrile. Each eluate was concentrated and analyzed by HPLC with multiwavelength detector. Recoveries of the pesticides in the overall procedure of this method were 78–114% for filtered river water and 75–107% for suspended solids. The limits of detection in water and suspended solids ranged from 0.1 to 0.9 μg/L and 1 to 7 μg/g, respectively. Pesticide distribution between soluble phase and suspended phase in river water was measured by this method.     

Determination of chlorothalonil residues in coffee

Coffee beans were treated with the fungicide chlorothalonil (2,4,5,6‐tetrachloro‐1,3‐benzene‐dicarbonitrile) and the residues were determined by high‐performance liquid Chromatograph (HPLC). Several techniques including Soxhlet extraction (SE), microwave‐assisted extraction (MAE) and accelerated solvent extraction (ASE) were compared for the extraction of residues. A column clean‐up procedure was developed to remove the co‐extractives in the extract before HPLC analysis. The overall mean recoveries from extracts obtained by SE, MAE and ASE were 89.2 ±3.9, 88.4 ±1.9 and 82.8 ±0.3, respectively. The results show that MAE followed by HPLC is a viable alternative to the commonly used SE and gas Chromatographic analysis for the determination of chlorothalonil in coffee.     

A rapid determination of histamine and 3-methylhistamine in human plasma by high performance liquid chromatography

Histamine plays an important pathophysiological role in allergy, inflammation, gastric acid secretion, microcirculation and neurotransmission. 3-Methylhistamine is a prominent metabolite of histamine. Different methods for determination of histamine in biological fluids have been developed. In the present study, a simple, simultaneous determination of histamine and 3-methylhistamine by HPLC (precolumn derivatization with fluorescamine) was developed in human plasma using fluorescence detection with 1-methylhistamine as the internal standard. Linear regression analysis of the ratios of the concentrations of histamine and 3-methylhistamine (X) against peak height ratios (Y) yielded the following: y = 0.0073x ? 0.0096 (R ² = 0.990) and y = 0.0077x ? 0.0111 (R ² = 0.989). In conclusion, it was possible to detect histamine and 3-methylhistamine below 5 ng mL^?1 in 1 mL plasma.     

Substitution of toxicologically critical solvents in the residue analysis of acetamiprid: Towards green chemistry

The article presents the reduced use of toxicologically critical solvents for the extraction and clean-up of a neo-nicotinoid pesticide, acetamiprid from vegetables. Acetamiprid was extracted from spiked vegetable samples of cabbage by the use of different techniques like microwave-assisted extraction (MWAE), sonication and by the conventional method of homogenization. The study revealed that though higher percent recoveries of 78–92 were obtained in the blending method, solvent use was high as compared to MWAE. In MWAE, the percent recoveries recorded were in the range of 46–89 depending upon the solvent used and power employed. A mixture of methanol–water and methanol–acetone at 400 W power levels gave percent recoveries of 72 and 82, respectively, as compared to solvent mixtures, namely, acetone–hexane and acetone–hexane–water, which recorded recoveries of 49 and 67%. The study indicates that the choice of solvent and power employed plays a significant role in MWAE for enhanced recoveries.     

Persistence of oxyfluorfen in soil and detection of its residues in rice crop

Oxyfluorfen is a post-emergence herbicide used for control of annual and perennial broad-leaf weeds and sedges in rice. There is increasing concern about persistence of pesticide residues in soils, agricultural products and sub-sequent contamination of ground water through runoff, leaching and drift. Thus, persistence of oxyfluorfen was evaluated under field conditions in a rice cropping system. Oxyfluorfen was sprayed at 240 and 500 g ai ha^?1 application rates to the rice crop as post-emergence herbicide. Paddy grains, straw and soil samples were collected at harvest and analyzed for oxyfluorfen residues by HPLC. Straw samples contained 0.01 and 0.03 µg g^?1 oxyfluorfen residues at 240 and 500 g ha^?1 concentrations, respectively. In the soil, 0.028 and 0.03 µg g^?1 of oxyfluorfen residues were detected when applied at 240 and 500 g ai ha^?1, respectively. However, in rice grains, 0.018 and 0.106 µg g^?1 of oxyfluorfen residues were found in 240 and 500 g ai ha^?1 treated plots. In light of the potential adverse effects of oxyfluorfen, it is important to determine herbicide levels in these crops.     

Polycyclic aromatic hydrocarbons in Syrian olive oils and their likely daily intakes

The levels of 16 US Environmental Protection Agency polycyclic aromatic hydrocarbons (16 EPA PAHs) in Syrian olive oils have been determined. Forty-two samples including commercial extra virgin and virgin olive oils, and virgin olive oils from olive mills were analyzed. Only naphthalene (NAP) was detected in all olive oil samples under investigation. Among the studied 16 EPA PAHs, the highest maximum concentration was also observed for NAP (120 μg kg^?1). Moreover, three samples exceeded the European Union (EU) maximum level of 2 μg kg^?1 for benzo[a]pyrene (BaP) in oils and fats, and only one sample exceeded the EU maximum level of 10 μg kg^?1 for the sum of benz[a]anthracene, chrysene, BaP, and benzo[b]fluoranthene (PAH4). The likely daily intakes of the total sum of 16 EPA PAHs, the sum of eight genotoxic PAHs, the sum of PAH4, the BaP, and the BaP equivalent through consumption of Syrian olive oils were estimated.