Key Laboratory of Agro-product Quality and Safety, Institute of Quality Standards & Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences, Beijing, 100081, China.
Agricultural and Rural Affair Bureau, Fengnan District, Tangshan City, Hebei Province, 063300, China.
J Chromatogr A. 2021 Jul 19;1649:462227. doi: 10.1016/j.chroma.2021.462227. Epub 2021 May 7.
A robust and confirmative method was established for the determination of six acetylgestagen residues, namely, flurogestone acetate (FGA), megestrol (MA), melengestrol acetate (MGA), chlormadinone acetate (CMA), medroxyprogesterone (MPA), and hydroxyprogesterone acetate (HPA) in animal-derived matrix samples by utilizing enhanced matrix removal lipid (EMR-lipid) clean-up in combination with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The analytes were extracted with acetonitrile, purified with a EMR-lipid cartridge, and separated with a reversed-phase C18 column. The limit of quantification (S/N ≥ 10) for CMA, FGA, HPA, MA, and MGA in all matrices was 0.5 ng/g, and for MPA, it was 1.0 ng/g; the limit of detection (S/N ≥ 3) for CMA, FGA, HPA, MA, and MGA in all matrices was 0.1 ng/g, and for MPA, it was 0.2 ng/g. The recoveries were between 61.0% and 114.8%, and the relative standard deviations (RSDs) were below 12%. The method was calibrated in a matrix-assisted standard solution in various linear ranges for the analytes and matrices, and the correlation coefficients (R) exceeded 0.99 for all the matrices.
建立了一种用于测定动物源性基质样品中六种乙酰基孕激素残留（醋酸氟孕酮（FGA）、美仑孕酮（MA）、醋酸甲地孕酮（MGA）、醋酸氯地孕酮（CMA）、醋酸甲羟孕酮（MPA）和羟孕酮醋酸酯（HPA））的可靠确证方法，该方法结合增强基质去除脂质（EMR-lipid）净化和超高效液相色谱-串联质谱法（UPLC-MS/MS）。用乙腈提取分析物，用 EMR-lipid 小柱纯化，用反相 C18 柱分离。所有基质中 CMA、FGA、HPA、MA 和 MGA 的定量限（S/N≥10）为 0.5ng/g，MPA 的定量限为 1.0ng/g；所有基质中 CMA、FGA、HPA、MA 和 MGA 的检测限（S/N≥3）为 0.1ng/g，MPA 的检测限为 0.2ng/g。回收率在 61.0%至 114.8%之间，相对标准偏差（RSD）低于 12%。该方法在基质辅助标准溶液中进行校准，适用于各种分析物和基质的线性范围，所有基质的相关系数（R）均超过 0.99。
