同位素稀释质谱法测定蜂蜜中4种硝基呋喃代谢物

Rapid determination of four nitrofuran metabolites in honey by isotope dilution-tandem mass spectrometry

研究了蜂蜜中4种硝基呋喃代谢物：呋喃唑酮代谢物（AOZ）、呋喃它酮代谢物（AMOZ）、呋喃妥因代谢物（AHD）、呋喃西林代谢物（SEM）的同位素稀释HPLC-MS／MS分析方法，以邻硝基苯甲醛作为衍生化试剂，AOZ-d4、AMOZ-d5、AHD-^13C3SEM·HCl-（^13C，^15N2）作内标，并将超声波衍生化法应用到实际样品的分析测试当中，以乙腈-0．1％甲酸为流动相，采用梯度洗脱，15min可将4种代谢物完全分离，再以MS，MS进行定性和定量分析。加标回收率为82％-112％；定量限（LOQ）为0．05—1ug／kg；检出限（IDD）为0．01～0．25ug／kg。该方法满足欧盟（EU）对进出口蜂蜜中硝基呋喃代谢物的检测要求。

A method for the determination of four nitroflLran metabolites such as 3-amino-2-oxazolidinone （AOZ）, 5- morpholinomethyl-3-amino-2-oxazolidinone （AMOZ）, 1-aminohydantoin （AHD）, and semicarbazide in honey has been established by isotope dilution high performance liquid chromatography-tandem mass spectrometry. Samples were derived with 2-nitrobenzaldehyde and （AOZ-d4） d4-3-amino-2-oxazolidinone, and ds-5-morpholinomethyl-3-amino-2- oxazolidinone （AMOZ-d5）, 13C isotope of 1-aminohydantoin （AHD-^13C3）, ^13C and ^15N isotope of semicarbazide （SEM·HCI-^13C ^15N2 ） were used as internal standards. Extracted with ultrasonic, the analytes were separated and analysed by gradient elution of acetonitrile and 0.1% formic acid in 15 min. The average recoveries were 82% - 112%; limits of quantification （LOQ） of 0.05 - 1ug/kg and limits of detection （LOD） of 0.01 -0.25 ug/kg were achieved using tandem mass spectrometry. All of the analytical results satisfied the detection demands of European Union for nitrofuran metabolites in import ＆ export honey.