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
2014年
11期
3467-3475
,共9页
李勇%林燕奎%李莉%颜治%王丙涛
李勇%林燕奎%李莉%顏治%王丙濤
리용%림연규%리리%안치%왕병도
海产品%锡形态分析%液相色谱法%原子荧光
海產品%錫形態分析%液相色譜法%原子熒光
해산품%석형태분석%액상색보법%원자형광
marine product%stannum speciation analysis%high performance liquid chromatography%atomic fluorescence spectrometry
目的:建立液相色谱串联原子荧光光谱仪检测海产品中不同形态的锡的测定方法。方法选择合适的提取液和流动相乙腈(v)∶水(v)∶乙酸(v)∶三乙胺(v)=65∶23∶12∶0.005来提高三甲基锡、一丁基锡、二丁基锡和三丁基锡的提取效率和分离度。通过调整灯电流、负高压、载气和屏蔽气流量以及还原剂的浓度,优化原子荧光检测条件,使待测物的荧光强度达到最佳状态。结果本方法的三甲基锡、一丁基锡、二丁基锡和三丁基锡在10~100μg/L范围内有良好的线性,方法的测定低限均为0.05 mg/kg;实验表明方法对不同海产品的回收率为81.5%~95.7%,相对标准偏差为1.0%~5.1%。结论该方法简便、准确,所使用的设备价格低廉,可用于海产品中4种锡形态的测定。
目的:建立液相色譜串聯原子熒光光譜儀檢測海產品中不同形態的錫的測定方法。方法選擇閤適的提取液和流動相乙腈(v)∶水(v)∶乙痠(v)∶三乙胺(v)=65∶23∶12∶0.005來提高三甲基錫、一丁基錫、二丁基錫和三丁基錫的提取效率和分離度。通過調整燈電流、負高壓、載氣和屏蔽氣流量以及還原劑的濃度,優化原子熒光檢測條件,使待測物的熒光彊度達到最佳狀態。結果本方法的三甲基錫、一丁基錫、二丁基錫和三丁基錫在10~100μg/L範圍內有良好的線性,方法的測定低限均為0.05 mg/kg;實驗錶明方法對不同海產品的迴收率為81.5%~95.7%,相對標準偏差為1.0%~5.1%。結論該方法簡便、準確,所使用的設備價格低廉,可用于海產品中4種錫形態的測定。
목적:건립액상색보천련원자형광광보의검측해산품중불동형태적석적측정방법。방법선택합괄적제취액화류동상을정(v)∶수(v)∶을산(v)∶삼을알(v)=65∶23∶12∶0.005래제고삼갑기석、일정기석、이정기석화삼정기석적제취효솔화분리도。통과조정등전류、부고압、재기화병폐기류량이급환원제적농도,우화원자형광검측조건,사대측물적형광강도체도최가상태。결과본방법적삼갑기석、일정기석、이정기석화삼정기석재10~100μg/L범위내유량호적선성,방법적측정저한균위0.05 mg/kg;실험표명방법대불동해산품적회수솔위81.5%~95.7%,상대표준편차위1.0%~5.1%。결론해방법간편、준학,소사용적설비개격저렴,가용우해산품중4충석형태적측정。
Objective To establish a method for determination of four different stannum species in ma-rine products by high performance liquid chromatography-atom fluorescent spectrometry (HPLC-AFS). Methods The solution which contained 65% acetonitrile, 23% water, 12% acetic acid and 0.005% three trie-thylamine was used to increase the extraction efficiency of trimethytin (TMT), monobutyltin (MBT), dibutyltin (DBT) and tributyltin (TBT), and to be the optimized mobile phase. The lamp current, negative high voltage, velocity of carrier gas, velocity of auxiliary gas, and concentrations of reducing agent were also optimized.Results The linear ranges for TMT, MBT, DBT and TBT were all from 10 to 100μg/L. The de-tection limits of TMT, MBT, DBT and TBT were 0.05 mg/kg. The recoveries of the method were 81.5%~95.7% (n= 8), and the relative standard deviations were 1.0%~5.1%.Conclusion This method is simple and convenient, and can be used to analyze the four stannum species in marine products.