液相色谱串联质谱法测定进出口水产品中亚甲基蓝药物残留

Determination of Methylene Blue Drug Residues in Import and Export Aquatic Products by Liquid Chromatography-Tandem Mass Spectrometry

运用高效液相色谱–电喷雾电离源串联四极杆质谱(HPLC-ESI(+)-MS/MS)法对进出口水产品中亚甲基蓝药物残留进行高灵敏分析。样品经过乙腈溶剂提取后,用中性氧化铝柱固相萃取柱化,洗脱收集后蒸干,残留用定容液溶解并过0.45 µm滤膜过滤,样品溶液供液相色谱–串联质谱仪测定。用HPLC-MS/MS在正离子模式下进行多反应监测(MRM)测定,根据校准曲线和外标法定量。电喷雾电离源正离子MRM模式检测:m/z 285.1/ 269.1;285.1/241.0。方法测定低限(LOQ, S/N >10)为0.1 μg/kg;线性范围:0.5~50 μg/L内峰面积与浓度成良好线性(R2 >0.999)。方法平均回收率范围在87.6%~111.2%,RSD范围在4.0%~10.2%。

In this study, a HPLC-ESI(+)-MS/MS methodology is used for the high sensitive determination of drug resi- due of methylene blue (MB) in import and export aquatic products. The sample was extracted by the acetonitrile and operated with a neutral alumina column solid-phase extraction column. After elution, it was evaporated to dryness. The residue was dissolved by constant volume liquid and was filtered through 0.45-µm membrane. The sample solution was for determination of liquid chromatography-tandem mass spectrometry. The liquid chromatography tandem mass spec- trometry was operated in the positive ion mode, using multiple reaction monitoring (MRM) for qualitative and quantita- tive analysis according to the calibration curve and the external standard method. Samples were detected with a ESI positive mode detector at MRM: m/z 285.1/269.1 and m/z 285.1/241.0. In the line of quality assurance, the stated LOQ of methylene blue residues in the negative sample was at the level of 0.1 µg/kg. The response for methylene blue was linear in the range of 0.5 - 50.0 μg/L, and the correlation coefficient is excellent 0.999. The average recovery range of this method was 87.6% - 111.2%, and the range of RSD was 4.0% - 10.2%.