| 液相色谱-串联质谱法测定水产品中亮绿、亚甲基蓝及其代谢物残留量 |
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| 基金项目:农业国家、行业标准制定和修定项目(农办质［2017］ 25号) |
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| 中文摘要:建立了水产品中亮绿、亚甲基蓝及其代谢物残留量同时测定的液相色谱-串联质谱(LC-MS/MS)方法。样品经乙酸铵缓冲溶液和乙腈提取，二氯甲烷液液萃取，PRS固相萃取柱净化，氮吹浓缩，定容后测定。以2 mmol/L乙酸铵(含01%甲酸)、乙腈和甲醇为流动相，CAPCELL PAK C18色谱柱进行分离，在选择反应监测(SRM)模式下测定，外标法定量。在最佳实验条件下，5种化合物在1.0~100.0 μg/L范围内线性关系良好(r2＞0.999)，检出限(LOD，S/N≥3)均为1.0 μg/kg，定量下限(LOQ，S/N≥10)均为2.0 μg/kg；在水产品中加标水平为1.0、5.0、10.0 μg/kg时，回收率为70.3%~92.1%，相对标准偏差(RSD，n=6)为2.3%~13%。该方法灵敏度高，能有效检测水产品中亮绿、亚甲基蓝及其代谢物的残留量。 |
| 中文关键词:亮绿 亚甲基蓝 代谢物 水产品 液相色谱-串联质谱(LC-MS/MS) |
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| Determination of Brilliant Green,Methylene Blue and Their Metabolites in Aquatic Products by Liquid Chromatography-Tandem Mass Spectrometry |
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| Abstract:A liquid chromatography-tandem mass spectrometric(LC-MS/MS) method was developed for the determination of brilliant green,methylene blue and their metabolites in aquatic products.The samples were extracted with ammonium acetate buffer solution and acetonitrile,followed by extraction with dichloromethane,then purified on a PRS solid phase extraction column.The eluent was concentrated by nitrogen blowing,diluted to a certain volume and determined.The targets were separated on a CAPCELL PAK C18 column with 2 mmol/L aqueous ammonium acetate containing 01% formic acid,acetonitrile and methanol as mobile phases.The determination of the analytes was performed by LC-MS/MS in selected reaction monitoring(SRM) mode,and the external standard method was used for quantitation.There existed good linear relationships for the analytes in the range of 10-100.0 μg/L with their correlation coefficients(r2) larger than 0.999.The limits of detection(LOD,S/N≥3) and quantitation(LOQ,S/N≥10) were 1.0 μg/kg and 2.0 μg/kg,respectively.The average recoveries at three spiked levels of 1.0,5.0 and 10.0 μg/kg were in the range of 70.3%-92.1% with their relative standard deviations(RSDs,n=6) of 23%-13%.The method has high sensitivity and could be used in the effective detection on residues of brilliant green,methylene blue and their metabolites in aquatic products. |
| Key Words:brilliant green methylene blue metabolites aquatic products liquid chromatography-tandem mass spectrometry(LC-MS/MS) |
| 引用本文：余玮玥，黄冬梅，史永富，孔聪，田良良，韩峰，张政权.液相色谱-串联质谱法测定水产品中亮绿、亚甲基蓝及其代谢物残留量[J].分析测试学报,2019,38(1):58-63. |
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