SPE-HPLC-MS/MS测定梨中多抗霉素B和宁南霉素残留

Determination of Polyoxin B and Ningnanmycin Residues in Pear by SPE-HPLC-MS/MS

[目的]建立固相萃取-高效液相色谱-串联质谱(SPE-HPLC-MS/MS)同时测定梨中多抗霉素B和宁南霉素残留的分析方法。[方法]样品用0.2%甲酸水提取,经HLB和MCX固相萃取柱净化上机。用Waters ACQUITY UPLC BEH Amide色谱柱分离,以0.1%甲酸和0.1%甲酸乙腈溶液为流动相进行梯度洗脱,多反应离子监测模式(MRM)扫描,以基质匹配标准曲线外标法定量。[结果]多抗霉素B和宁南霉素在0.005~0.2 mg/L的质量浓度范围内均呈现良好的线性关系(R2>0.999);在0.02、0.5、2.0 mg/kg的3个加标水平下,回收率为77%~91%,相对标准偏差(RSD)为2.8%~5.8%。[结论]该方法易于操作,灵敏度高,适用于梨中多抗霉素B和宁南霉素残留的同时检测。

[Aims]This study aims to establish an analytical method for simultaneous determination of polyoxin B and Ningnanmycin residues in pear by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry(SPE-HPLC-MS/MS).[Methods]The sample was extracted with a formic acid solution 0.2%,purified by HLB and MCX solid phase extraction column.The chromatographic analysis was performed on a Waters ACQUITY UPLC BEH Amide column using gradient elution with a formic acid solution 0.1%and formic acid acetonitrile 0.1%as mobile phases,finally analyzed in multiple reaction monitoring(MRM)mode and quantified by matrix-matched standard curve external standard method.[Results]The results showed that there is a good linear relationship for polyoxin B and ningnanmycin in the range of 0.005-0.2 mg/L(R2>0.999).The recoveries at three spiked levels(0.02,0.5,2.0 mg/kg)for both compounds ranged from 77 to 91%,with relative standard deviations(RSD)of 2.8-5.8%.[Conclusions]Due to easy operation and highly sensitivity,the method is suitable for simultaneous detection of polyoxin B and ningnanmycin residues in pear.