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气相色谱-串联质谱法测定台湾青枣中炔螨特、戊唑醇和溴螨酯农药残留量

[Determination of propargite, tebuconazole and bromopropylate pesticide residues in Taiwan green jujubes by gas chromatography-tandem mass spectrometry].

作者信息

Zhang Qun, Liu Chunhua, Wu Nancun, Wu Xiaofang, Li Shuhuai

出版信息

Se Pu. 2014 Aug;32(8):886-9. doi: 10.3724/sp.j.1123.2014.04014.

Abstract

An analytical method was established for the determination of propargite, tebuconazole and bromopropylate in Taiwan green jujubes (Zizyphus mauritiana Lam) by gas chromatography-tandem mass spectrometry (GC-MS/MS). The sample was extracted with acetonitrile from the Taiwan green jujubes after treated with a homogenizer. The organic phase was then separated from water phase by adding NaCl. The extract was further purified on a carbon/ NH2 cartridge with elution solvents of acetonitrile/toluene (3:1, v/v). Finally, the target analytes were separated by a capillary gas chromatographic column SLB-5MS (30 m x 0. 25 mm x 0. 25 μm). A tandem quadrupole mass spectrometer operated in either full scan mode or in MS/MS mode for multiple reaction monitoring (MRM) was used for the qualitative and quantitative analysis of the constituents, respectively. The results showed that the average recoveries of the three pesticides ranged from 75. 8% to 103. 6% with the RSDs of 1. 7%-9. 3% at the spiking levels from 0.01 mg/kg to 0. 50 mg/kg (n= 5). The calibration curves showed good linearity in the range of 0.01-0.50 mg/kg, with the determination coefficients over 0.99 (R2>0.99). The limits of quantification (LOQs) were 0.01 mg/kg for propargite, tebuconazole and bromopropylate in Taiwan green jujubes. The method is available for the determination of propargite, tebuconazole and bromopropylate pesticide residues in Taiwan green jujubes.

摘要

建立了一种气相色谱 - 串联质谱法(GC - MS/MS)测定台湾青枣(毛叶枣)中炔螨特、戊唑醇和溴螨酯的分析方法。将台湾青枣经匀浆器处理后用乙腈进行提取。通过加入氯化钠使有机相与水相分离。提取物再经碳/氨基柱净化,以乙腈/甲苯(3:1,v/v)作为洗脱溶剂。最后,目标分析物通过SLB - 5MS毛细管气相色谱柱(30 m×0.25 mm×0.25μm)进行分离。分别使用串联四极杆质谱仪在全扫描模式或多反应监测(MRM)的MS/MS模式下对成分进行定性和定量分析。结果表明,在0.01 mg/kg至0.50 mg/kg的加标水平下(n = 5),三种农药的平均回收率在75.8%至103.6%之间,相对标准偏差为1.7% - 9.3%。校准曲线在0.01 - 0.50 mg/kg范围内呈良好线性,决定系数大于0.99(R²>0.99)。台湾青枣中炔螨特、戊唑醇和溴螨酯的定量限均为0.01 mg/kg。该方法可用于测定台湾青枣中炔螨特、戊唑醇和溴螨酯的农药残留。

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