| 固相萃取-柱后衍生-反相高效液相色谱法测定脱水蒜粉中的亚硫酸盐 |
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| 引用本文： | 徐琴,王凤美,牟志春,赵华梅,刘琳.固相萃取-柱后衍生-反相高效液相色谱法测定脱水蒜粉中的亚硫酸盐[J].分析试验室,2009,28(10). |
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| 作者姓名： | 徐琴 王凤美 牟志春 赵华梅 刘琳 |
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| 作者单位： | 山东出入境检验检疫局技术中心,青岛,266002 |
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| 摘 要： | 建立了测定脱水蒜粉中亚硫酸盐含量的柱后衍生-反相高效液相色谱分析方法.样品用HCl/甘露醇缓冲溶液提取,经固相萃取(SPE)小柱净化本底并富集待测物后,与甲醛缓冲液反应生成稳定的化合物羟甲基磺酸盐,采用高效液相色谱柱及柱后衍生分离,紫外检测器检测,外标法定量.色谱柱为:Agila Venusil MP-C18(4.6 mm×250 mm),流动相为0.005 mol/L四丁基氢氧化铵离子溶液(pH 4),检测波长为450 nm,结果表明,检出限为2.0 mg/kg,在0.1～10.0 μg/mL范围内线性关系良好,相关系数R2=0.9998,样品添加回收率为86.5%～97.6%,RSD为2.2%～4.0%(n=5).
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| 关 键 词： | 脱水蒜粉 亚硫酸盐 固相萃取 柱后衍生 反相高效液相色谱 |
Determination of sulfite in dehydrated garlic using high performance liquid chromatography with post-column derivatization |
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| XU Qin,WANG Feng-mei,MU Zhi-chun,ZHAO Hua-mei,LIU Lin.Determination of sulfite in dehydrated garlic using high performance liquid chromatography with post-column derivatization[J].Chinese Journal of Analysis Laboratory,2009,28(10). |
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| Authors: | XU Qin WANG Feng-mei MU Zhi-chun ZHAO Hua-mei LIU Lin |
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| Institution: | Technology Center for Shandong Entry-Exit Inspection and Quarantine Bureau of China;Qingdao 266002 |
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| Abstract: | A new high performance liquid chromatographic method with post-column detection for the determination of sulfite in dehydrated garlic was developed.Sulfite in dehydrated garlic was extracted with HCl/mannitol solution,and then the extract was cleaned up and enriched on a C18 solid-phase extraction column.By adding formaldehyde sulfite was converted to hydroxymethylsulfonate(HMS).HMS can be determined by high performance liquid chromatography with post-column detection.An agila venusil MP-C18 column was equi... |
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| Keywords: | Dehydrated garlic Sulfite High performance liquid chromatography Solid phase extraction Post-column detection |
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