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31.
气相色谱-质谱大体积进样法测定蔬菜、水果中17种农药残留 总被引:4,自引:0,他引:4
建立了GC—MS/SIM与大体积进样技术结合测定蔬菜、水果中包括有机磷类、氨基甲酸酯类、有机氯类、菊酯类在内的17种农药的方法。样品经丙酮提取,OASIS HLB固相萃取小柱净化后,采用GC—Ms的选择离子模式和大体积进样技术进行测定,能够使相对检出限降低1~2个数量级。大多数农药的线性范围为0.05~10mg/kg,相关系数为0.9943—0.9996,相对标准偏差为3.5%-10.3%,回收率范围在77%~107%之间.方法能满足果蔬中17种农残限量的的检测要求,具有灵敏、快速、重复性好的特点。 相似文献
32.
A molecular dynamics study of the dark adapted visual pigment rhodopsin molecule was carried out. The interaction of the chromophore
group, 11-cis-retinal, with the nearest amino acid residues in the chromophore center of the molecule, namely, in the region of the protonated
Schiff base linkage, was analyzed. Most likely, the interaction of the CH=NH bond with the negatively charged amino acid residue
Glu113 cannot be described as a simple electrostatic interaction of two oppositely charged groups. One can propose that not
only Glu113 but also Glu181 and Ser186 are involved in stabilization of the protonated Schiff base linkage. Accord-ing to
calculations, Glu181 interacts, as the counter-ion, with the Schiff base indirectly via Ser186. The intramolecular mechanisms of protonated Schiff base stabilization in rhodopsin are discussed.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 19–27, January, 2007. 相似文献
33.
Summary A gas chromatographic methodology with selective detection is presented for the analysis in wines and corks of pentachlorophenol residues, which are suspected to be the most likely precursors of some off-flavours described in several wine samples. After derivatisation, pentachlorophenol acetate residues were monitored by electrolytic conductivity detection and/or mass spectrometric detection in the selective ion mode at m/z 264 and 266. Recoveries varied from 80 to 96% for wine samples fortified with 5 to 100 g l–1 and from 83 to 91% for corks (fortified at 25 to 100 g kg–1). The proposed methodology allowed for a determination limit of g l–1 for wine and 10 g kg–1 for corks. 相似文献
34.
A fast multi‐residue screening method for determining pesticides in tea is described. Pesticides are extracted from tea with acetone and methylene chloride, then enriched and cleaned up with solid phase extraction (SPE) prior to gas chromatographic determination. The fast screening is achieved by a gas chromatograph system equipped with dual‐column, dual‐tower auto‐sampler and both electron capture detector (ECD) and flame photometric detector (FPD). Optimal conditions are investigated for the prospective pesticides including column selection, detection mode, the retention behaviors, quantitative calibration, as well as the recoveries and repeatability of pesticides from tea samples. Under the optimal conditions, with the FPD‐P detector accompanied CP‐SIL 13CB column, 48 pesticides can be separated well and detected within 38 min; and with a DB‐5 column, 35 ECD‐detectable pesticides can be separated and detected within 46 min. The recoveries of 84 pesticides in tea samples are 65–120% with 0.34–16% RSD for spiking 0.02–3.0 mg/kg standard species. Because of the thermal instability of most pesticides, direct cold extraction of pesticides from a tea sample is recommended. The proposed method provided a very fast and efficient procedure to screen 84 pesticides from a complicated tea sample matrix. 相似文献
35.
A simple method is described for the quantitative determination of organochlorine pesticides and polychlorinated biphenyls (PCB's) in water at the sub-ppb level. A micro gas-phase extractor advantageously replaces other preconcentration and purification techniques. The extract is analyzed by capillary gas chromatography without further enrichment. The recovery at the ppb level was nearly 100% for organochlorine pesticides and more than 80% for PCB's. The complete procedure including sample preparation, steam distillation-extraction, and capillary gas chromatographic analysis is carried out in less than four hours. 相似文献
36.
Jiantao Fu Zihao Li Rilin Huang Shiying Wang Congling Huang Dongmei Cheng 《International journal of environmental analytical chemistry》2016,96(14):1367-1377
Two independent field trials were conducted in Guangdong and Guangxi, South China, in 2013, to study the dissipation, residue levels, and distribution of pyraclostrobin in banana and soil under field conditions. Pyraclostrobin residues were determined through a quick and effective method of high-performance liquid chromatography. Results showed that the average recoveries ranged from 80.55% to 98.08%, with relative standard deviations of 3.18–7.81% at three different spiking levels for each different matrix. The quantification limit of the proposed method was 0.006 mg/kg for both banana and soil. The half-lives of pyraclostrobin in bananas were 9.09 days in Guangdong and 8.26 days in Guangxi, and both bananas exhibited a dissipation rate of 90% after 28 days. The half-lives of pyraclostrobin in soil were 11.61 days in Guangdong and 10.60 days in Guangxi, with a dissipation rate of 90% after 35 days. Although several positive banana samples (i.e., pyraclostrobin exceeding the maximum residue limits (MRL) were found, the terminal residues in banana pulp were not detectable. All the terminal residues in banana pulp were below the MRL of 0.02 mg/kg, set by the Chinese Ministry of Agriculture, indicating a negligible risk associated with the exposure to pyraclostrobin via the consumption of banana. The distribution of pyraclostrobin in soil was also investigated in two experimental sites. The pyraclostrobin in different layer soil was time dependent and did not vary between the two sites. The result also showed that pyraclostrobin could be easily transported from the top soil to the subsoil. However, the highest quantity ratio did not exceed 10% in the bottom layer (20–30 cm). The distribution assessment also revealed that no significant potential environment risk was induced by pyraclostrobin in bananas. 相似文献
37.
M. T. Lafuente J. L. Tadeo 《International journal of environmental analytical chemistry》2013,93(1-2):99-108
Abstract The determination of imazalil and prochloraz fungicide residues has been carried out by HPLC with an UV detector at 204 nm and by GLC with an electron capture detector (ECD). In both cases fungicide residues were extracted with hexane/acetone (90:10, v/v) after pH adjustment and purified by a liquid-liquid partitioning process. When HPLC was used for prochloraz and imazalil analysis, it was necessary to eliminate the interfering substances with a further clean-up process. This was also required when samples with low residue levels were analyzed by GLC. Recovery was always higher than 70%. The detection limit was 0.04 ppm for the HPLC method and 0.02 for the GLC method. Imazalil and prochloraz residues in “Washington Navel” oranges and “Hernandina” clementine fruits, dipped in a 1000 ppm fungicide solution, are reported. 相似文献
38.
《Journal of separation science》2018,41(5):1083-1090
A method based on ultra‐high performance liquid chromatography was developed and validated to detect six thyreostatic compounds: tapazole, thiouracil, methylthiouracil, dimethylthiouracil, propylthiouracil, and phenylthiouracil in faeces of bovine. Thyreostats were extracted from the matrix with a mixture of methanol and buffer (pH = 8). Next step was derivatization of analytes with 3‐iodobenzylbromide. The liquid chromatographic separation of derivatives was obtained on a SB‐C18 column (50 × 2.1 mm; 1.8 μm, Agilent) with gradient elution using a mobile phase consisting of acetonitrile/0.1% acetic acid within 7.5 min. The analysis was performed on a Shimadzu NEXERA X2 ultra‐high performance liquid chromatograph with triple quadrupole MS 8050 instrument operating in positive electrospray ionization mode. Depending on the target compound, two or three diagnostic signals (selected reaction monitoring transitions) were monitored. The procedure was validated according to the Commission Decision 2002/657/EC. Recovery and repeatability met the performance criteria specified by this document for banned compounds. The recovery ranged from 97.5 to 110.5%, and repeatability did not exceed 14.1%. Decision limits and detection capabilities were below 10 μg/kg. The highest decision limits and detection capabilities concentrations were observed for phenylthiouracil of 3.48 and 6.96 μg/kg, respectively. 相似文献
39.
Thanh Duc Mai Benjamin Bomastyk Hong Anh Duong Hung Viet Pham Peter C. Hauser 《Analytica chimica acta》2012
An extension of a capillary electrophoresis instrument coupled to a sequential injection analysis manifold was developed for automated measurements with on-line solid-phase extraction preconcentration. An in-house built capacitively coupled contactless conductivity detector was employed for sensitive detection with narrow capillaries of 25 μm internal diameter. The system was assembled into standardized 19 in. frames and racks for easy transport and mobile deployment. The system can be left running unattendedly without manual intervention with good operation stability. To demonstrate the application of the system, a method for the determination of four drugs, namely ibuprofen, diclofenac, naproxen and bezafibrate, was developed with enrichment factors of up to several hundreds. Detection of the drug residues down to the nM-scale was found possible and the method was found suitable for the detection of ibuprofen in the waste water of a hospital in Hanoi. 相似文献
40.
J. D. Macneil J. R. Patterson A. C. Fesser C. D. Salisbury S. V. Tessaro C. Gates 《International journal of environmental analytical chemistry》2013,93(1-2):145-153
Abstract Tissue samples were collected from ten healthy mature female wood bison (B. bison athabascae) for examination. Livers and kidneys were tested for toxic heavy metals and trace metals considered as essential nutrients for successful reproduction, while fat samples were analyzed for persistent chlorinated hydrocarbons. No elevated levels of toxic heavy metals (arsenic, cadmium, lead, mercury) were found and essential trace elements (copper, manganese, selenium, zinc) were within the acceptable ranges established for healthy cattle. All fat samples tested contained trace levels of α-BHC (mean value, 23 ppb) and lindane (mean value, 3 ppb). 相似文献