超高效液相色谱-质谱法测定有机农药制剂中烷基酚聚氧乙烯醚
Determination of Alkylphenol Ethoxylates in Organic Pesticides by UPLC-MS
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摘要: 建立了超高效液相色谱-质谱法(UPLC-MS)测定乳油、微乳剂、悬浮剂、水乳剂、可溶液剂和水剂6类有机农药液体制剂中辛基酚聚氧乙烯醚和壬基酚聚氧乙烯醚的含量。样品经甲醇超声辅助提取，稀释后采用BEH C18色谱柱(2.1 mm×100 mm×1.7 μm)分离，以10 mmol/L乙酸铵溶液和甲醇为流动相，梯度洗脱，柱温为30 ℃，流速为0.3 mL/min，电喷雾电离正离子模式，选择离子监测(SIR)模式定量。结果表明，辛基酚聚氧乙烯醚(OPEO)和壬基酚聚氧乙烯醚(NPEO)在50~10 000 μg/L浓度范围内的线性关系良好(r＞0.999)，在5、20、100 mg/kg添加水平内的添加回收率为81.8%~115.5%，相对标准偏差为1.1%~9.8%，两种化合物的定量限均为50 μg/L。该方法操作简便、快速、准确、稳定性好，适用于有机农药中烷基酚聚氧乙烯醚类助剂的定性分析和定量检测。
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关键词:
- 超高效液相色谱-质谱(UPLC-MS) /
- 有机农药 /
- 农药助剂 /
- 烷基酚聚氧乙烯醚
Abstract: A method of ultra performance liquid chromatography-mass spectrometry (UPLC-MS) was established for the determination of octylphenol ethoxylates and nonylphenol ethoxylates in six kinds of liquid organic pesticides formulations (emulsifiable concentrate, microemulsion, suspension concentrate, emulsion in water, soluble concentrate and aqueous solutions). The samples were ultrasonic extracted and diluted with methanol，then separated by Waters BEH C18 column (2.1 mm×100 mm×1.7 μm) with 10 mmol/L ammonium acetate and methanol as mobile phase, gradient elution and column temperature of 30 ℃, while the flow rate was 0.3 mL/min. Quantification was performed in selected ion record (SIR) mode using Quattro Premier XE mass spectrometer with positive ion mode of electrospray ionization. The results showed that the octylphenol ethoxylates (OPEO) and nonylphenol ethoxylates (NPEO) in the concentration range of 50-10 000 μg/L have good linear relationships (r>0.999). The recoveries at three spiked levels (5, 20, 100 mg/kg) are 81.8%-115.5% (n=8) with the relative standard deviation of 1.1%-9.8% (n=8), and the limit of quantitative is 50 μg/L. The method is simple, rapid, accurate, and which is suitable for qualitative analysis and quantitative detection of alkylphenol ethoxylates additives in organic pesticides. -
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