用高效液相色谱-串联质谱法测定水产品中硝基呋喃代谢物的含量.样品经稀盐酸水解并用2-硝基苯甲醛(2-NBA)衍生,调节其酸度至pH 7.0~7.5,离心,将上清液过Oasis HLB(6 mL)小柱后,以乙酸乙酯为洗脱剂,将洗脱液于40 ℃在氮气流中挥干,并用乙腈与乙酸(1+99)溶液以体积比3比7混合的溶液溶解.用氘代试剂内标法定量.硝基呋喃代谢物标准的质量浓度在4.5 μg·L-1以内呈线性,回收率在80.2%~98.4%之间,相对标准偏差(n=8)在3.75%~8.12%之间,测定限(10S/N)为0.25 μg·kg-1.

In this paper,a method of HPLC-MS-MS for the determination of nitrofuran metabolites in aquatic products was proposed.The sample was hydrolyzed with dilute hydrochloric acid then derivatized with 2-nitrobenzene formaldehyde (2-NBA).The derivatized solution was adjusted to pH 7.0-7.5 then separated by centrifugation.The supernatant was introduced into the Oasis HLB microcolumn (6 mL) and eluted with ethyl acetate.The eluate was dried in a nitrogen flow at 40 ℃,and dissolved with a mixture of acetonitrile and acetic acid (1+99) which were mixed in the ratio of 3 to 7 by volume.The metabolites were determined by HPLC-MS/MS using deuterium reagent as internal standard.Linearity of the calibration curves was in the range within 4.5 μg·L-1.Determination limit (10S/N) of the method was 0.25 μg·kg-1.Recovery was ranged from 80.2% to 98.4%,and RSD′s (n=8) from 3.75% to 8.12%.