| 高效液相色谱－串联质谱法测定水产品中9种禁用染料类药物残留 |
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| 基金项目:海关总署科研计划项目（2020HK225）；湛江市科技计划项目（2012E0202） |
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| 中文摘要:建立了高效液相色谱－串联质谱（HPLC－MS/MS）测定水产品中亮绿、亚甲基蓝及其3种代谢物、孔雀石绿、隐性孔雀石绿、结晶紫与隐性结晶紫共9种禁用染料类物质的方法。样品搅碎后用乙腈-0.1 mol/L乙酸铵（pH 4.5）提取，提取液经氯化钠盐析萃取，正己烷液液萃取和PRS柱固相萃取净化，氮吹浓缩后进行测定。采用Luna C18（2.1 mm × 50 mm，5 μm）色谱柱进行分离，乙腈和5 mmol/L乙酸铵（含0.1%甲酸）为流动相梯度洗脱，多反应监测（MRM）正离子电离模式下测定，采用外标法定量。9种待测物在0.5 ~ 20.0 μg/L范围内呈良好线性关系，相关系数（r2）均大于0.99，检出限（LOD）均为0.5 μg/kg，定量下限（LOQ）均为1.0 μg/kg。以罗非鱼、金鲳鱼、南美白对虾和青蟹为空白基质，在0.5、1.0、5.0 μg/kg加标水平下，平均加标回收率为76.8% ~ 104%，相对标准偏差（RSD，n = 7）为4.3% ~ 10%。采用该方法检测经亚甲基蓝药浴的罗非鱼样品，检出亚甲基蓝与天青B。该方法准确、可靠，重现性好，可用于水产品中9种禁用染料类药物的定量分析。 |
| 中文关键词:高效液相色谱－串联质谱（HPLC－MS/MS） 禁用染料类药物 水产品 |
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| Determination of 9 Kinds of Banned Dye Drugs in Aquatic Products by High Performance Liquid Chromatography－Tandem Mass Spectrometry |
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| Abstract:A high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS） method was developed for the determination of nine banned dyes in aquatic products，including bright green，methylene blue and its three metabolites，malachite green and leucomalachite green，crystal violet and leucocrystal violet．After pretreatment procedure，samples were extracted with acetonitrile－0.1 mol/L ammonium acetate（pH 4.5） solution．Extract solution were purified by salt-out extraction of sodium chloride，n-hexane and PRS solid phase extraction column．The targets were separated on a Luna C18（2.1 mm × 50 mm，5 μm） column with a mobile phase consisting of acetonitrile-5 mmol/L ammonium acetate（0.1% formic acid） for gradient elution．Mass spectrometry multiple reaction monitoring（MRM） and positive ion ionization mode were used for testing and external standard method was used for quantitative analysis．Good linear relationships were obtained for nine compounds in the content range of 0.5－20.0 μg/L，with correlation coefficients（r2） greater than 0.99．The limits of detection（LODs）were 0.5 μg/kg，and limits of quantitation（LOQs）were 1.0 μg/kg．Tilapia，pomfret，shrimp and crab were used as the blank matrix，and spiked at the levels of 0.5，1.0，5.0 μg/kg．The average recoveries were 76.8%－104%，and the relative standard deviations（RSDs，n = 7） were 4.3%－10%．By using this method，methylene blue and azure B were detected in tilapia samples which were treated with methylene blue medicine bath．The method is accurate，reliable and reproducible，so it can be used for the quantitative analysis of 9 banned dyes in aquatic products. |
| Key Words:high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS） banned dyes drugs aquatic products |
| 引用本文：孙良娟，李红权，蔡润斌，庄姜云，唐庆强，唐媛媛，钟键，黄武.高效液相色谱－串联质谱法测定水产品中9种禁用染料类药物残留[J].分析测试学报,2023,(1):89-95. |
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