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  • yolk

    第15楼2008/09/03

    你好,我要怎样才能防止乳化呢?

    watericecat 发表:这个方法,第一注意液液萃取的时候不要乳化,一旦乳化结果就不好了。第二,也是最重要的一点,ph调节的时候一定要精确,否则做不出回收率的。

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  • 第16楼2008/09/03

    适当增大溶剂量,加入石油醚的同时加入饱和氯化钠溶液。振荡充分即可,别太久。一旦乳化,加溶剂或者加盐破乳。

    yolk 发表:你好,我要怎样才能防止乳化呢?

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  • 我在故我思

    第18楼2009/02/06

    Determination of carbendazim, thiabendazole, and o-phenylphenol residues in lemons by HPLC following sample clean-up by ion-pairing
    Konstantinos P. Prousalis, et al.;
    Analytical and Bioanalytical Chemistry, Volume 379, Number 3/2004: 458-463

    Abstract:
    An efficient analytical method is presented involving effective sample clean-up with solid-phase extraction and HPLC-UV analysis for the simultaneous determination of carbendazim, thiabendazole, and o-phenylphenol residues in lemons. Sample preparation involves extraction with acetonitrile acidified with trifluoroacetic acid and an ethyl acetate/petroleum ether mixture. Purification of the crude extract was carried out with liquid–liquid partitioning after addition of an aqueous ammonia solution. Final clean-up was performed on polymeric reversed-phase cartridges pretreated with sodium dodecyl sulfate. Chromatographic analysis was performed on a reversed-phase HPLC column isocratically eluted with an acetonitrile/water/ammonia mixture and UV detection at 254 nm. The chromatographic method is repeatable, reproducible, and sensitive. Fungicide recoveries from lemon samples fortified at levels of 5 and 1 mg kg–1 were 81–85% for carbendazim, 96–98% for thiabendazole, and 81–106% for o-phenylphenol with coefficients of variation of 2.5–7.4%. Detection limits for carbendazim, thiabendazole, and o-phenylphenol in lemons were 0.21, 0.27, and 0.51 mg kg–1, respectively.
    http://www.springerlink.com/content/mab4q3yc1bkkeff4/




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  • 我在故我思

    第19楼2009/02/06

    Determination of carbendazim, thiabendazole and thiophanate-methyl in banana (Musa acuminata) samples imported to Italy
    Food Chemistry,Volume 87, Issue 3, September 2004,383-386
    Attilio Veneziano,et al.;

    Abstract:
    The occurrence of benzimidazole fungicides (benomyl and its metabolites carbendazim, thiabendazole and thiophanate-methyl) in 50 banana samples imported to Italy from Ecuador, Panama and Costa Rica during 2002–2003 was investigated. In 11 samples, thiabendazole was found at concentrations ranging from 0.050 to 2.510 mg/kg. In five samples, carbendazim was found at concentrations ranging from 0.140 to 1.100 mg/kg, whereas thiophanate-methyl was not detected in any sample. Analysis was carried out using HPLC-DAD and positive samples were confirmed by GC–MS. Recoveries of carbendazim, thiabendazole and thiophanate-methyl at four fortification levels (0.5, 1.0, 2.5 and 4.0 mg/kg) were in the range 81–96% for carbendazim and thiabendazole and 63.2–69.8% for thiophanate-methyl. Only two samples contained carbendazim that exceeded the FAO/WHO Codex Alimentarius and the Italian Department of Health maximum residue limits.


    http://www.sciencedirect.com/science?_ob=ArticleURL&_udi=B6T6R-4BRSFK9-6&_user=10&_rdoc=1&_fmt=&_orig=search&_sort=d&view=c&_acct=C000050221&_version=1&_urlVersion=0&_userid=10&md5=4ea8d8b2f228f6214f6a0f5207b2df12

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  • christinazy

    第21楼2013/04/12

    最近我也在做多菌灵的方法,貌似,多菌灵的单标做液相都是两个峰。流动相分别用甲醇:磷酸盐缓冲溶液(ph6.8),甲醇:磷酸,甲醇:离子对试剂,甲醇:水这4种,比值都是40:60,信号是280nm,全部都出来2个峰,这是为什么?请问到底做多菌灵液相应该用哪种流动相最合适?才能防止甲基菌硫灵出现?

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  • yolk

    第22楼2013/05/03

    现在我们用LC-MSMS做多菌灵检测了,回收率很好

    cowboy20052005(cowboy20052005) 发表:请问现在有没有合适的前处理方法了?谢谢。。。。。。最近我也在做多菌灵,且回收率一直很低很低。。。。。。

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  • 该帖子已被版主-雾非雾加2积分,加2经验;加分理由:信息反馈。能说说前处理方法么?
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  • crystaltao

    第23楼2013/09/18

    我用少量盐酸溶解多菌灵,然后用甲醇定容。再做标准曲线,流动相甲醇和水对半,只有一个峰。特征波长258nm

    christinazy(christinazy) 发表:最近我也在做多菌灵的方法,貌似,多菌灵的单标做液相都是两个峰。流动相分别用甲醇:磷酸盐缓冲溶液(ph6.8),甲醇:磷酸,甲醇:离子对试剂,甲醇:水这4种,比值都是40:60,信号是280nm,全部都出来2个峰,这是为什么?请问到底做多菌灵液相应该用哪种流动相最合适?才能防止甲基菌硫灵出现?

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  • xndxlzm

    第24楼2013/09/20

    应助达人

    可以考虑用液质做,前处理用已经提取,Qsechers方法净化,效果还是不错的

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