
LC-MS/MS测定3种复合蔬果汁中吡唑醚菌酯、啶虫脒及哒螨灵残留
Pyraclostrobin, Acetamiprid and Pyridaben Residues in Three Composite Fruit and Vegetable Juice: Determination by LC-MS/MS
为了探究目前蔬果生产中常用杀菌剂、杀虫剂、杀螨剂在复合蔬果汁中的残留情况,本研究建立了3种复合蔬果汁中吡唑醚菌酯、啶虫脒和哒螨灵残留的LC-MS/MS分析方法。选取以不同蔬果进行调和的3种复合蔬果汁为材料,采用含1%(v%)乙酸的乙腈溶液提取,以SPE-NH2柱进行净化,以C18色谱柱分离待测物,采用电喷雾离子化,正离子扫描和多反应监测模式(MRM)检测,基质匹配标准溶液外标法定量。试验结果表明:啶虫脒在5~1000 μg/L,吡唑醚菌酯和哒螨灵在1~500 μg/L范围内均有良好的线性关系,相关系数(R2)在0.9984以上。添加浓度为0.010、0.10和0.50 mg/kg时,3种复合蔬果汁中吡唑醚菌酯、啶虫脒及哒螨灵回收率为80.6%~113.4%;相对标准偏差(RSD)介于0.5%~9.3%之间;以最低添加浓度0.010 mg/kg为方法定量限(LOQ)。该方法快捷、简便、准确,满足复合蔬果汁中吡唑醚菌酯、啶虫脒及哒螨灵残留分析的要求。
In order to explore the residues of fungicides, insecticides and acaricides, which are commonly used in fruit and vegetable planting, in composite fruit and vegetable juice, a method for the simultaneous detection of pyraclostrobin, acetamiprid and pyridaben in 3 kinds of composite fruit and vegetable juice by LC-MS/MS was developed. Three composite fruit and vegetable juice made by mixed vegetables and fruits were selected as the materials. The samples were initially extracted by acetonitrile containing 1% (v%) acetic acid, and cleaned up by SPE-NH2 column. The targets were separated on a C18 column, and detected by LC-MS/MS with ESI positive polarity multiple reactions monitoring (MRM) mode. The matrix-matched external standard calibration curves were used for quantitative analysis. The results showed that: good linear relationship appeared in 5-1000 μg/L of acetamiprid and 1-500 μg/L of pyraclostrobin and pyridaben. The correlation coefficients (R2) were higher than 0.9984. Under three spiked levels of 0.010, 0.10 and 0.50 mg/kg, the recovery rates ranged from 80.6% to 113.4%, and the relative standard deviations (RSD) were 0.5%-9.3%. Limit of quantification (LOQ) of pyraclostrobin, acetamiprid and pyridaben were 0.010 mg/kg, which was the lowest spiked concentration. The method can meet the requirements for the determination of pyraclostrobin, acetamiprid and pyridaben residues in composite fruit and vegetable juice simultaneously, and it is quick, efficient and accurate.
蔬果汁 / 吡唑醚菌酯 / 啶虫脒 / 哒螨灵 / 残留 {{custom_keyword}} /
fruit and vegetable juice / pyraclostrobin / acetamiprid / pyridaben / residue {{custom_keyword}} /
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