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Simultaneous determination of clanobutin, dichlorvos, and naftazone in pork, beef, chicken, milk, and egg using liquid chromatography-tandem mass spectrometry
Food Chemistry ( IF 8.5 ) Pub Date : 2018-01-12 , DOI: 10.1016/j.foodchem.2018.01.085
Jin-A. Park , A.M. Abd El-Aty , Weijia Zheng , Seong-Kwan Kim , Sang-Hyun Cho , Jeong-min Choi , Ahmet Hacımüftüo , Ji Hoon Jeong , Jing Wang , Jae-Han Shim , Ho-Chul Shin

A chromatographic method involving a single run was validated for the quantification of clanobutin, dichlorvos, and naftazone in products of animal origin. Pork, beef, chicken, milk, and egg samples were extracted with a solution of 0.1% formic acid in acetonitrile, defatted with n-hexane, centrifuged, and filtered prior to analysis using liquid chromatography-tandem mass spectrometry (LC-/MS/MS). The analytes were separated on a C18 column using a solution of 0.1% formic acid and 10 mM ammonium formate (A) and acetonitrile (B) as the mobile phase. A good linearity over 5–50 ng/g concentration range was obtained with coefficients of determination (R2) ≥ 0.9807. The intra- and interday accuracy (recovery %) calculated from 3 fortification levels (5, 10, and 20 ng/g) were 73.2–108.1% and 71.4–109.8%, and the precisions (expressed relative standard deviations (RSDs)) were 0.9–12.9% and 1.8–10.6%, respectively, for the 3 tested analytes in animal originated foods. The limits of quantification (LOQs) ranged between 0.1 and 1 ng/g, thus enabling the quantification of residual levels below the uniform maximum residue limit (MRL) of 0.01 mg/kg set for compounds having no MRL. The designated methodology was successfully applied to monitor various samples collected from Seoul; the tested analytes were not quantified in any of the market samples. Conclusively, the developed method is simple, sensitive, and accurate, and could be used for the detection of pharmaceuticals in various animal food matrices with variable protein and fat contents.



中文翻译:

液相色谱-串联质谱法同时测定猪肉,牛肉,鸡肉,牛奶和鸡蛋中的黑色素,敌敌畏和那夫zone

验证了涉及单次运行的色谱方法,用于定量动物源性产品中的盐酸克拉布丁,敌敌畏和纳法酮。猪肉,牛肉,鸡肉,牛奶,鸡蛋和样品用0.1%甲酸的乙腈溶液中的溶液萃取,用脱脂Ñ己烷,离心,并用液相色谱-串联质谱(LC-/ MS分析之前过滤/多发性硬化症)。使用0.1%甲酸和10 mM甲酸铵(A)和乙腈(B)的溶液作为流动相,在C18色谱柱上分离分析物。在5–50 ng / g的浓度范围内,具有良好的线性,并具有测定系数(R 2)≥0.9807。由3个设防水平(5、10和20 ng / g)计算得出的日内和日间准确度(回收率%)为73.2–108.1%和71.4–109.8%,准确度(表示为相对标准偏差(RSD))为在动物源性食品中测试的3种分析物分别为0.9–12.9%和1.8–10.6%。定量限(LOQ)在0.1 ng / g和1 ng / g之间,因此可以对残留水平进行定量,该水平低于无MRL化合物设定的0.01 mg / kg的统一最大残留限量(MRL)。指定的方法已成功应用于监测从首尔收集的各种样品;被测分析物未在任何市场样品中进行定量。最终,所开发的方法简单,灵敏,准确,

更新日期:2018-01-12
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