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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

DOI: 10.12677/HJFNS.2013.24014, PP. 73-77

Keywords: 水产品；亚甲基蓝；液相色谱–串联质谱法；残留
Aquatic Products, Methylene Blue (MB), LC-ESI(+)-MS/MS, Residues

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Abstract:

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

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