海参和海参苗种中硝基呋喃类代谢物残留的液质联用检测法

Determination of nitrofuran metabolites in sea cucumber and fingerlings by high performance liquid chro-matography-tandem mass spectrometry

优化了液相色谱-串联质谱法测定海参和海参苗种中硝基呋喃类代谢物残留量的检测方法。样品经酸解、衍生和乙酸乙酯萃取、浓缩后,以1mL20%的甲醇-水溶液定容,采用液相色谱-三重四级杆串联质谱仪、多反应监测扫描模式(MRM)检测和同位素内标法定量。4种硝基呋喃类代谢物检测的线性范围为0.5～10.0ng/mL,定量限为0.5μg/kg。在加标量为2.5μg/kg时,样品加标回收率范围为90.8%～99.0%,相对标准偏差(RSD)小于10%,满足硝基呋喃类药物的检测要求。

In this study, we optimized a high performance liquid chromatography -tandem mass spectrometric （HPLC -MS/MS） method for determining 4 nitrofuran metabolites in sea cucumber and fingerlings, namely 1 - aminohydantoin hydrochloride （AHD） ,3 - amino - 5 - morpholinomethyl - 2 - oxazolidineone （ AMOZ）, 3 - ami- no- 2 - oxazolidinone （AOZ） and semicarbazide （SEM）. Samples were subjected to HC1 acidolysis, derivation, ethyl acetate extraction, concentration and constant volume with methanol solution （CH3 OH ： H2O = 20 ： 80） pri- or to HPLC -MS/MS analysis. The analysis was carried out in the multi -reaction monitoring （MRM） mode and internal standard isotope dilution method was used for quantification. Calibration curves for the analytes exhibited good linearity over the concentration range from 0.5 to 10.0 ng/mL and their limits of quantification were all 0. 50μg/kg. The range of average recoveries for them was from 90.8% - 99.0% with an amount of 2. 50μg/kg standard addition. And relative standard deviation （RSD, n = 5） is less than 10%. The method can meet the re- quirements of detection for 4 nitrofuran metabolites in sea cucumber and fingerlings.