固相萃取-液相色谱-串联质谱法快速测定饲料中氯羟吡啶含量的研究OA

To address the problems of low sensitivity,cumbersome pretreatment,large matrix interference,and easy missed detection of low concentration of clopidol in feed,this study aimed to establish a solid-phase extraction-liquid chromatography-tandem mass spectrometry(SPE-LC-MS/MS)method for the rapid determination of clopidol content in feed,in order to meet the requirements of accurate quantification and safety supervision.Clopidol in feed samples was extracted using a 0.2%ammonia-methanol solution,purified through an alkaline alumina solid-phase extraction(SPE)cartridge,and separated on a C18 column with gradient elution using ammonium formate solution and methanol as the mobile phase.Detection was performed by LC-MS/MS in positive electrospray ionization(ESI+)mode,and quantification was conducted using matrix-matched external standard calibration.The results showed that clopidol exhibited a good linearity within the concentration range of 0.2-100 μg/L,with a correlation coefficient(r2)greater than 0.999.The method detection limits(LOD)and quantification limits(LOQ)were 0.05 mg/kg and 0.1 mg/kg,respectively.Method accuracy was evaluated in various types of feed,yielding recoveries of 90%-102%,with a relative standard deviation(RSD)below 7%.This analytical method is simple to perform,highly sensitive,accurate,and reproducible,and significantly improves the detection limit and qualitative reliability compared with the national standard method.It meets the methodological requirements for the determination of clopidol in feed and provides a reliable technical approach for its precise quantification.