| DSPE-HPLC-MS法测定水产品中的三聚氰胺 |
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| 引用本文： | 杨玉秀,黄和,廖建萌,黄国方,谢丽玲,罗林. DSPE-HPLC-MS法测定水产品中的三聚氰胺[J]. 食品与机械, 2012, 28(3): 71-75 |
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| 作者姓名： | 杨玉秀 黄和 廖建萌 黄国方 谢丽玲 罗林 |
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| 作者单位： | 1. 广东海洋大学食品科技学院,广东湛江,524025
2. 广东省湛江市质量计量监督检测所,广东湛江,524043 |
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| 摘 要： | 建立分散固相萃取-高效液相色谱质谱联用法测定水产品中三聚氰胺的方法。样品用甲醇、pH 4.5的乙酸铵缓冲溶液提取,分散固相萃取净化。经Thermo Fisher Hyper-sil Gold C18柱(150mm×2.1mm,5μm)分离,选择反应监测(SRM)正离子模式测定。结果表明,三聚氰胺含量为5～50ng/mL时线性关系良好,其线性方程为Y=8 958.7 X-3 327.8,相关系数R2=0.999 6,检出限为0.01mg/kg,平均回收率在82.8%～100.4%,RSD均小于5.0%。
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| 关 键 词： | 三聚氰胺 分散固相萃取 高效液相色谱质谱联用法 水产品 |
Determination of melamine in aquatic products by high performance liquid chromatography-mass spectrometry with dispersive solid phase extraction |
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| YANG Yu-xiu , HUANG He , LIAO Jian-meng , HUANG Guo-fang , XIE Li-ling , LUO Lin. Determination of melamine in aquatic products by high performance liquid chromatography-mass spectrometry with dispersive solid phase extraction[J]. Food and Machinery, 2012, 28(3): 71-75 |
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| Authors: | YANG Yu-xiu HUANG He LIAO Jian-meng HUANG Guo-fang XIE Li-ling LUO Lin |
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| Affiliation: | 1.Institute of Food Science and Technology of Guangdong Ocean University,Zhanjiang,Guangdong 524025,China;2.Zhanjiang Institute of Supervision & Test on Quality & Measure,Zhanjiang,Guangdong 524043,China) |
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| Abstract: | A method for determination of melamine in aquatic products was established by high performance liquid chromatography-mass spectrometry(HPLC-MS).Samples were extracted with Methanol,in pH 4.5 by buffer solution of ammonium,and then cleaned with dispersive solid phase extraction.After extracted and separated on a Thermo Fisher Hypersil Gold C18(150 mm× 2.1 mm,5 μm), the analytes were detected by HPLC-MS with the selected reaction monitoring(SRM) mode.The calibration curves of melamine were linear in the range of 5 ng/mL~50 ng/mL form,the linear equation was Y = 8 958.7 X-3 327.8, the correlation coefficient was 0.999 6,the limit of quantization was 0.01 mg/kg,and the average recovery was in the range of 82.8% ~ 100.4%,RSD<5.0%. |
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| Keywords: | melamine dispersive solid phase extraction high performance liquid chromatography-mass spectrometry aquatic products |
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