固相萃取一毛细管柱气相色谱法测定韭菜中
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S816. 17

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Determination of phorate and its metabolite phorate sulfone in leek by solid phase extraction and capillary gas chromatography
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    摘要:

    目的建立一种固相萃取一毛细管柱气相色谱法测定韭菜中甲拌磷及其代谢物甲拌磷砜含量的方法。方 法样品经乙腈提取后,用C18、PC/NH7固相萃取柱对样品提取净化,用DB一1701毛细管柱气相色谱法进行测定。 结果 当样品中分别添加甲拌磷和甲拌磷砜为0. 03、0.30、0.90和3.00 mg/kg时,甲拌磷的平均回收率为 86. 7%~ 93. 2%,变异系数为2.46%~4.76%;甲拌磷砜的平均回收率为85. 9%~ 92. 5%,变异系数为2.82%~ 4. 31%。该方法检出限为0.01 mg/kg,仪器检出限为0.01 ng。结论 该法快速、准确、检测限低、精密度高,适用 于韭菜中甲拌磷和甲拌磷砜的检测。

    Abstract:

    Objective To estahlish a solicl phase extraction/capillary gas chromatography ( SPE-GC) method t。 determine phorate and its metabolite phorate sulfone residue in leek. Methods After being extractecl by acetonitrile, samples were further extracted and purified by C18 and PC/NH2 solid-phase extraction columns and then detected by capillary gas chromatography with DB-1701 column. Results As 0. 03 , 0. 30, 0. 90 and 3. 00 mg/kg of both phorate and phorate sulfone being added to samples, average recoveries of phorate ranged from 86. 7% t0 93. 2% , and its coefficients of variation ranged from 2. 46% t0 4. 76%. Average recoveries of phorate sulfone ranged from 85. 9% t0 92. 5% and its coefficients of variation ranged from 2. 82% t0 4. 31% . The limit of detection of the method was 0. 01 m~kg and the limit of quantitation was 0. 01 ng. Conclusion The ruethod is rapid, accurate, sensitive and low in determination limit, thus applicable in the detection of phorate and phorate sulfone in leek.

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张以春,雍宗锋.固相萃取一毛细管柱气相色谱法测定韭菜中[J].中国食品卫生杂志,2012,24(1):34-36.

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