Over the past few decades, honey products have been polluted by different contaminants, such as pesticides, which are widely applied in agriculture. In this work, a modified EN – quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method was developed for the simultaneous quantification of pesticide residues, including cymiazole, fipronil, coumaphos, fluvalinate, amitraz, and its metabolite 2,4-dimethylaniline (2,4-DMA), in four types of honey (acacia, wild, chestnut, and manuka) and royal jelly. Samples were buffered with 0.2 M dibasic sodium phosphate (pH 9), and subsequently, acetonitrile was employed as the extraction solvent. A combination of primary secondary amine (PSA) and C18 sorbents was used for purification prior to liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI⁺/MS-MS) analysis. The estimated linearity measured at six concentration levels presented good correlation coefficients (R²) ≥ 0.99. The recovery, calculated from three different spiking levels, was 62.06–108.79% in honey and 67.58–106.34% in royal jelly, with an RSD < 12% for all the tested compounds. The matrix effect was also evaluated, and most of the analytes presented signal enhancement. The limits of quantification (LOQ) ranged between 0.001 and 0.005 mg/kg in various samples. These are considerably lower than the maximum residue limits (MRL) set by various regulatory authorities. A total of 43 market (domestic and imported) samples were assayed for method application. Among the tested samples, three samples were tested positive (i.e. detected and quantified) only for cymiazole residues. The residues in the rest of the samples were detected but not quantified. We concluded that the protocol developed in this work is simple and versatile for the routine quantification of cymiazole, 2,4-DMA, fipronil, coumaphos, amitraz, and fluvalinate in various types of honey and royal jelly.

在过去的几十年中，蜂蜜产品已被各种污染物（例如农药）污染，这些污染物已广泛应用于农业。在这项工作中，开发了一种改良的EN –快速，简便，廉价，有效，坚固耐用且安全的（QuEChERS）提取方法，用于同时定量测定农药残留，包括cymiazole，fipronil，coumaphos，fluvalinate，Amitraz及其代谢物2 ，4-二甲基苯胺（2,4-DMA），存在四种类型的蜂蜜（洋槐，野生，栗子和麦卢卡）和蜂王浆中。样品用0.2 M磷酸氢二钠（pH 9）缓冲，然后，将乙腈用作萃取溶剂。在液相色谱-电喷雾串联质谱（LC-ESI）之前，使用伯仲胺（PSA）和C18吸附剂的组合进行纯化⁺ / MS-MS）分析。在六个浓度水平下测得的估计线性呈现出良好的相关系数（R ²）≥0.99。从三种不同的加标水平计算得出，蜂蜜中的回收率为62.06-108.79％，蜂王浆中的回收率为67.58-106.34％，所有测试化合物的RSD <12％。还评估了基质效应，大多数分析物均表现出信号增强作用。在各种样品中，定量限（LOQ）介于0.001和0.005 mg / kg之间。这些大大低于各种监管机构设定的最大残留限量（MRL）。总共对43种市场（国内和进口）样品进行了分析，以用于方法应用。在测试样品中，仅对氰基咪唑残留物测试了三个样品呈阳性（即检测和定量）。检测到其余样品中的残留物，但未进行定量。