高效液相色谱-串联质谱法测定水产品中红霉素的残留

Determination of erythromycin residue in fishery products by high performance liquid chromatography-tandem mass spectrometry

研究了水产品中红霉素残留量测定的新方法。该方法以红霉素同位素标记物(Erythromycin,N,N-Dimethyl-13 C2)为内标物,样品用乙腈提取、正己烷净化。分析条件为:以Hypersil C18为色谱分离柱,甲醇和0.1mmol/L乙酸为流动相,用带有电喷雾离子源的三重四极杆串联质谱测定,内标法定量。红霉素在添加量0.5～20.0μg/kg的范围内,回收率为87.0%～97.8%,相对标准偏差小于10%,方法检出限为0.5μg/kg。

A method was developed for the determination of erythromyein residue in fishery products. The erythromycin isotope label was used as the internal standard. The samples were extracted with acetonitrile and the sample extracts were purified by n-hexane. The erythromycin was separated on a C18 column with a binary mobile phase of methnol and 0. 1 mmol/L acetic acid, analyzed by a triple quadrupole tandem mass spectrometer via electrospray ionization source （ESI） and quantified by the internal standard method. The recoveries of erythromycin were in the range of 87.0% - 97.8% with spiked levels of 0.5- 20.0μg/kg. The RSD was less than 10%. The detection limits was 0.5μg/kg.