GC-MS/MS同时检测圆葱、辣根中122种农药残留

Simutaneous determination method of 122 pesticides residues in onion and horseradish by gas chromatography triple quadrupole tandem mass spectrometry

以气相色谱三重四极串联质谱仪（GC-MS/MS）为检测手段,建立了复杂基质圆葱、辣根中122种农药残留的同时检测方法。改进并优化了前处理方法：在40mL乙酸乙酯∶正己烷饱和的乙腈（15∶85,V∶V）的混合溶剂中加入5.0g醋酸钠,1%的冰乙酸,以此混合溶剂作为提取液,超声40min,40℃下浓缩;净化方法选用加入PSA（0.3g）及石墨化炭黑（0.3g）的QuEChERS法。本方法的最低检出限范围在0.000625～0.05mg/kg,122种农药在圆葱、辣根中的回收率范围为60.0%~130.6%,相对标准偏差为3.7%~29.8%。

A multi-residue method had been developed and validated for the simultaneous quantification and confirmation of 122 multiclass pesticides in complex matrix vegetables onion and horseradish by gas chromatography triple quadrupole tandem mass spectrometry （GC-MS/MS）. The pretreatment was developed and optimized： samples were extracted with the solution （40mL） of ethyl acetate and acetonitrile （hexane saturated） （15 ：85, V ：V） containing 1% of acetic acid and 5g of sodium acetate,followed by the treatment of ultrasound （40min）. Primary secondary amine （PSA, 0.3g） and GCB （0.3g） were applied for purification simutaneously to achieve quick, easy,cheap, effective, rugged and safe analysis. A final concentration step at 40~C was included in order to increase sensitivity in the instrumental analysis. The limit of dectection for this method was 0.000625-0.05mg/kg. Recoveries of 122 multiclass pesticides were studied in onion and horseradish,yielding values in the range 60.0%N130.6% with precision values,expressed as relative standard deviation（RSD） of 3.7%N29.8%.