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【求助】关于输日蔬菜新增11项农药检验方法

农残检测

  • 我们新接到通知要求输日冷冻蔬菜新增11项农药检测项目:解毒喹、氯酯磺草胺、氯虫酰胺、氯磺隆、百治磷、醚磺隆、磺酰磺隆、四氯苯酞、双氟磺草胺、双炔酰菌胺、甲磺隆,但找不到标准,如何检验。拜托帮忙一下!我们现有资源是两台气相色谱配备ECD、FPD、NPD检测器。
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  • sumzhou

    第1楼2009/04/16

    解毒喹、LC/MS/MS
    氯酯磺草胺、LC/MS/MS
    氯虫酰胺、不知道
    氯磺隆、LC/MS/MS
    百治磷、GC/MS
    醚磺隆、LC/MS/MS
    磺酰磺隆、不知道
    四氯苯酞、GC/MS
    双氟磺草胺、不知道
    双炔酰菌胺、不知道
    甲磺隆、LC/MS
    不知道的可能用LC/MS/MS吧,以您老哥的配置,百治磷、四氯苯酞可以试验一下

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  • realtiger

    第2楼2009/04/16

    大部分用液相,光有气相是不够的
    磺酰脲可以用液质质NY/T 1616-2008

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  • 我在故我思

    第3楼2009/04/17

    JAP-092 氯磺隆和甲磺隆检测方法
    http://down.foodmate.net/standard/sort/13/10317.html

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  • 我在故我思

    第5楼2009/04/17

    楼主,你好!以下的一些英文文献如果需要全文可以去文献求助应助版面求助。
    双氟磺草胺(florasulam)
    Determination of herbicides in mineral and stagnant waters at ng/L levels using capillary electrophoresis and UV detection combined with solid-phase extraction and sample stacking
    Javier Hernández-Borges,et al.;
    Journal of Chromatography A,Volume 1070, Issues 1-2, 8 April 2005, Pages 171-177
    Abstract:
    In this work, the combined use of solid-phase extraction (SPE) and on-line preconcentration strategies as normal stacking mode (NSM) and stacking with matrix removal (SWMR) for the ultrasensitive and simultaneous capillary electrophoresis-ultraviolet analysis (CE-UV) of five triazolopyrimidine sulfonanilide pesticides (i.e., diclosulam, cloransulam-methyl, flumetsulam, metosulam and florasulam) in different types of water is investigated. An adequate separation electrolyte for the separation and stacking of these pesticides was obtained, considering also its compatibility with MS detection, which consisted of 24 mM formic acid and 16 mM ammonium carbonate at pH 6.4. It was observed that the use of this running buffer together with the SWMR preconcentration method provided the best results in terms of sensitivity (between 6.54 and 11.9 μg/L) and peak efficiency (up to 550 000 theoretical plates per meter, NTP/m). When this on-line preconcentration procedure was combined with an off-line sample preconcentration step as SPE using C18 cartridges, the selected herbicides could be detected in the ng/L range. The optimized SPE-SWMR-CE-UV method was applied to the determination of the selected group of pesticides in spiked and non-spiked mineral and stagnant waters. Recoveries ranged between 55 and 110% and limits of detection between 131 and 342 ng/L. This work shows the great possibilities of the combined use of SPE-SWMR-CE-UV to overcome the sensitivity problems usually linked to CE analysis.
    http://www.sciencedirect.com/science?_ob=ArticleURL&_udi=B6TG8-4FMK8GJ-5&_user=1915929&_rdoc=1&_fmt=&_orig=search&_sort=d&view=c&_acct=C000055340&_version=1&_urlVersion=0&_userid=1915929&md5=cd3aca0e5791b2bb0ee7bc5f57d52eee

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  • 我在故我思

    第6楼2009/04/17

    双炔酰菌
    http://www.dbpia.co.kr/view/ar_view.asp?arid=1098539
    这个是朝鲜语的,有英文摘要,楼主可以参考一下。

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  • 我在故我思

    第7楼2009/04/17

    磺酰磺隆(sulfosulfuron)
    High performance liquid chromatographic method for residue determination of sulfosulfuron.
    Saha S, Singh SB, Kulshrestha G.
    J Environ Sci Health B. 2003 May;38(3):337-47

    A method was developed for sulfosulfuron [(1-(2-ethylsulfonylimidazo [1,2-a] pyridin-3-ylsulfonyl)-3-(4,6-dimethoxy pyrimidin-2yl)] and its three major metabolites by HPLC utilizing photodiode array detector. The method makes use of Lichrosphere RP-8 column and acetonitrile:water:orthophosphoric acid (80:20:0.1 v/v/v) as mobile phase at a flow rate of 1 ml min(-1). Using these condition sulfosulfuron, and compounds II, III and IV were resolved with distinct Rt of 2.088, 2.216, 2.302 and 2.476 minutes, respectively. Sulfosulfuron residues were analysed in soil, wheat grain and straw samples by extracting with a mixture of acetonitrile and 2 M ammonium carbonate (100 ml, 9:1, v/v) using horizontal shaker for soil and Soxhlet apparatus for wheat grain and straw samples. The extracts were cleaned up by partitioning with dichloromethane in case of soil and hexane followed by dichloromethane for plant samples. The percent recovery ranged between 71 to 75.2 for soil and 70.8 to 74.7 for plant samples. The limit of determination of sulfosulfuron was 0.25 microg g(-1).
    http://www.ncbi.nlm.nih.gov/pubmed/12716051

    Determination of sulfosulfuron residues in soil under wheat crop by a novel and cost-effective method and evaluation of its carryover effect
    Singh, Shashi B | Kulshrestha, Gita
    Journal of Environmental Science and Health, Part B: Pesticides, Food Contaminants and Agricultural Wastes. Vol. 42, no. 1, pp. 27-31. Jan. 2007

    A novel and cost-effective method of sulfosulfuron extraction has been developed using distilled water as an extraction solvent. Using this method, the environmental fate of sulfosulfuron was investigated in soil under wheat crop. Studies were conducted under natural field conditions in randomized block design and herbicide (75% water dispersible granules (WG)) was applied after 24 days of sowing. The rates of applications were 25 and 50 g of active ingredient (a.i.) per hectare. Soil samples were collected at predetermined intervals and analyzed by high performance liquid chromatography (HPLC). The minimum detection limit was found to be 0.001 is a subset of g g- 1. The dissipation of sulfosulfuron followed first-order rate kinetics and dissipated with a half-life of 5.4-6.3 days. After harvest, field soil was used for conducting a pot experiment with bottle gourd (Lagenaria siceraria) as test plants to study the carry over effect of sulfosulfuron. No phytotoxicity was observed to bottle gourd in pot experiment with harvest soil.
    http://md1.csa.com/partners/viewrecord.php?requester=gs&collection=TRD&recid=08173550EN&q=&uid=1039883&setcookie=yes


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