摘要
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4.5μg·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0.25μg·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 · L^-1. Recovery was ranged from 80. 2^ to 98. 4^, and RSD＇s （n=8） from 3. 75% to 8. 12%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2008年第11期1028-1030,1034,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
浙江省分析测试基金资助项目的子课题
