食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
FOOD SAFETY AND QUALITY DETECTION TECHNOLOGY
2013年
6期
1853-1858
,共6页
尚德荣%秦德元%赵艳芳%翟毓秀%宁劲松%丁海燕%盛晓风%徐正
尚德榮%秦德元%趙豔芳%翟毓秀%寧勁鬆%丁海燕%盛曉風%徐正
상덕영%진덕원%조염방%적육수%저경송%정해연%성효풍%서정
高压液相色谱%氢化物发生原子荧光光谱%水产品%硒形态
高壓液相色譜%氫化物髮生原子熒光光譜%水產品%硒形態
고압액상색보%경화물발생원자형광광보%수산품%서형태
high performance liquid chromatography%hydride generation atomic fluorescence spectrome-try%aquatic products%selenium speciation
目的:采用高压液相色谱-氢化物发生-原子荧光光谱联用技术(HPLC-HG-AFS)对水产品中硒的赋存形态检测进行研究。方法通过实验优化流动相、提取剂、提取时间及其仪器条件,建立HPLC-HG-AFS联用技术检测水产品中硒形态的分析方法。用去离子水在70℃水浴下超声提取1 h,流动相为 pH 6.0的40 mmol/L(NH4)2HPO4溶液,阴离子交换柱分离, HG-AFS检测。结果样品加标量在0.10、1.00 mg/kg时的回收率均在86.6%以上,相对标准偏差均小于5%。结论本研究证明使用该方法测定水产品中的硒形态较为准确、可靠,为科学评价水产品质量、进一步细化富硒水产品的判定标准和鉴别其真伪提供技术手段,为科学有效地开展其风险评估提供技术支撑和数据支持。
目的:採用高壓液相色譜-氫化物髮生-原子熒光光譜聯用技術(HPLC-HG-AFS)對水產品中硒的賦存形態檢測進行研究。方法通過實驗優化流動相、提取劑、提取時間及其儀器條件,建立HPLC-HG-AFS聯用技術檢測水產品中硒形態的分析方法。用去離子水在70℃水浴下超聲提取1 h,流動相為 pH 6.0的40 mmol/L(NH4)2HPO4溶液,陰離子交換柱分離, HG-AFS檢測。結果樣品加標量在0.10、1.00 mg/kg時的迴收率均在86.6%以上,相對標準偏差均小于5%。結論本研究證明使用該方法測定水產品中的硒形態較為準確、可靠,為科學評價水產品質量、進一步細化富硒水產品的判定標準和鑒彆其真偽提供技術手段,為科學有效地開展其風險評估提供技術支撐和數據支持。
목적:채용고압액상색보-경화물발생-원자형광광보련용기술(HPLC-HG-AFS)대수산품중서적부존형태검측진행연구。방법통과실험우화류동상、제취제、제취시간급기의기조건,건립HPLC-HG-AFS련용기술검측수산품중서형태적분석방법。용거리자수재70℃수욕하초성제취1 h,류동상위 pH 6.0적40 mmol/L(NH4)2HPO4용액,음리자교환주분리, HG-AFS검측。결과양품가표량재0.10、1.00 mg/kg시적회수솔균재86.6%이상,상대표준편차균소우5%。결론본연구증명사용해방법측정수산품중적서형태교위준학、가고,위과학평개수산품질량、진일보세화부서수산품적판정표준화감별기진위제공기술수단,위과학유효지개전기풍험평고제공기술지탱화수거지지。
Objective The determination of selenium speciation in aquatic products by high performance liquid chromatography-hydride generation-atomic fluorescence spectrometry (HPLC-HG-AFS) was analyzed in this study. Methods The mobile phases, extraction reagents, extraction time and instrumental conditions were optimized and then selenium speciation in aquatic products was analyzed by HPLC-HG-AFS. Samples were extracted at 70℃for 1 h by ultrasonic extraction and the flow phase was 40 mmol/L (NH4)2HPO4 (pH6.0). The different selenium speciation was separated with anion exchange column and detected by HG-AFS. Results The average recoveries of 0.10 mg/kg and 1.00 mg/kg in samples were all above 86.6%and the relative stan-dard deviations were all below 5% with a high accuracy. Conclusion The established method was accurate and reliable for selenium speciation analysis. It could provide technological support for scientific evaluation of the aquatic product quality, as well as the authenticity of the selenium enriched aquatic products. At the same time, the method also could provide important information for risk assessment of the aquatic products.