固相萃取与高效液相色谱法快速测定猪肉中的三聚氰胺 |
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引用本文: | 马毅红,林海波,吕飞. 固相萃取与高效液相色谱法快速测定猪肉中的三聚氰胺[J]. 安徽农业科学, 2012, 0(6): 3583-3585 |
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作者姓名: | 马毅红 林海波 吕飞 |
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作者单位: | 1. 惠州学院化学工程系,广东惠州,516007 2. 惠州检验检疫局,广东惠州,516015 |
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摘 要: | [目的]研究高效液相色谱法测定猪肉中三聚氰胺含量的方法,加强食品和饲料中三聚氰胺的监控。[方法]猪肉样品经乙腈-水(7∶3,V/V)溶液提取,于OasisMCX固相萃取柱净化,采用高效液相色谱法测定猪肉中三聚氰胺的含量。[结果]确定仪器最佳工作条件为:流动相为乙腈-0.05 mol/L磷酸盐缓冲液(7∶3,V/V),流速为1.5 ml/min,柱温35℃,波长235 nm,进样量20μl。在此条件下,三聚氰胺在0.1~100.0 mg/L具有良好的线性关系,相关系数达0.999 89,对猪肉中三聚氰胺的检出限为0.5 mg/kg,在加标0.5~5.0mg/kg浓度范围内,回收率在86.0%~108.0%,相对标准偏差(RSD)小于7.4%。[结论]该方法操作简便、快速、灵敏、准确,适合于测定猪肉中的三聚氰胺。
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关 键 词: | 高效液相色谱法 固相萃取 猪肉 三聚氰胺 |
Rapid Determination of Melamine in Pork by Solid Phase Extraction and HPLC Method |
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Affiliation: | MA Yi-hong et al(Department of Chemical Engineering,Huizhou University,Huizhou,Guangdong 516007) |
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Abstract: | [Objective] The aim was to study determining melamine content in pork by using HPLC method,and strengthening monitor of melamine in food and feed.[Method]The pork sample was extracted by solution of methyl cyanide mixed with aqueous(7∶ 3,V/V),and purified by OasisMCX solid phase extraction column,the content of melamine in pork was determined by HPLC.[Result] The optimum working conditions were determined: methyl cyanide-0.05 mol/L phosphate buffer(7∶ 3,V/V),flow rate 1.5 ml/min,column temperature 35 ℃,wavelength 235 nm,injection volume 20 μl.Under this condition,melamine has good linear relationship at 0.1-100.0 mg/L,the correlation relationship is 0.999 89,the detection limit is 0.5 mg/kg.In the range of adding sample 0.5-5.0 mg/kg,the recovery rate is 86.0%-108.0%,RSD is less than 7.4%.[Conclusion]The method is easy,rapid,sensitive and accurate for determining melamine in pork. |
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Keywords: | High performance liquid chromatography(HPLC) Solid phase extraction Pork Melamine |
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