A method was developed for the confirmatory and quantitative analysis of one pyrethrin and 18 pyrethroid residues in animal fat. Fat was extracted was collected from adipose tissue melted in an oven at 65 °C for 2 h. Fat samples (1 g) were dispersed with deactivated Florisil^® sorbent and extracted with MeCN. Sample extracts were purified by cold temperature precipitation at −30 °C for 4 h and further purified using dispersive solid-phase extraction (d-SPE) clean-up in tubes containing 500 mg of Z-SEP+ and 125 mg of PSA bonded silica. Purified samples were analysed by ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC–MS/MS) detection. Chromatographic separation was carried out on a Acquity C₈ BEH column, using a binary gradient separation comprising of mobile phase A, 5 mM ammonium formate in water:MeOH (80:20, v/v,) and mobile phase B, 5 mM ammonium formate in MeOH. The mass spectrometer was operated in the positive electrospray ionisation mode (ESI(+)). Validation was performed following the 2002/657/EC guidelines. Trueness ranged between 84% and 143% and precision ranged between 3.9% and 29%. The developed method is particularly advantageous because the sample preparation procedure does not require complex sample extraction equipment and uses less solvent compared to other sample preparation protocols.

开发了一种方法用于动物脂肪中一种除虫菊酯和18种除虫菊酯残留的确证和定量分析。从在65°C的烤箱中融化2 h的脂肪组织中收集脂肪。脂肪样品（1克）分散失活硅酸镁^®吸附剂和用MeCN萃取。样品提取物通过在-30°C下冷沉淀4 h进行纯化，然后在包含500 mg Z-SEP +和125 mg PSA键合二氧化硅的试管中使用分散固相萃取（d-SPE）纯化进行进一步纯化。纯化的样品通过超高效液相色谱-串联质谱（UHPLC-MS / MS）检测进行分析。色谱分离是在Acquity C _{8上进行的}BEH色谱柱，使用二元梯度分离法，其中包括流动相A，在水：MeOH中的5 mM甲酸铵（80：20，v / v）和流动相B，在MeOH中的5 mM甲酸铵。质谱仪在正电喷雾电离模式（ESI（+））下运行。按照2002/657 / EC指南进行验证。真实度介于84％和143％之间，精度介于3.9％和29％之间。所开发的方法是特别有利的，因为与其他样品制备方案相比，样品制备过程不需要复杂的样品提取设备并且使用较少的溶剂。