Determination of Five Kinds of Mercury Species in Shrimp Feed by LC-AFS with Accelerated Solvent Extraction
摘 要
称取经粉碎的样品1.000 0 g,置于加速溶剂提取池中,加入10 mL的5 mol·L-1盐酸溶液、1 mL的5 mol·L-1氯化钾溶液和2 mL的10 mol·L-1半胱氨酸溶液;在8.0 MPa和70℃下,预加热2 min,加热5 min,静态提取5 min,分离,重复上述提取过程2次,合并提取液;加入0.2 mL的0.5 mol·L-1半胱氨酸溶液、1.5 mL的6 mol·L-1氢氧化钠溶液,以10 000 r·min-1离心5 min,将上清液氮吹浓缩并用硝酸(5+95)溶液定容至1 mL,过0.45 μm尼龙滤膜后,采用Eclipse XDB-C18反相色谱柱(150 mm×4.6 mm,5.0 μm)分离溶液中的甲基汞、乙基汞、无机汞、硫柳汞和苯基汞,流动相为50 g·L-1乙腈溶液+5 g·L-1乙酸铵溶液+1 g·L-1半胱氨酸溶液(体积比为1∶1∶1),用原子荧光光谱仪进行测定。5种形态的汞的质量浓度在一定范围内与其荧光强度呈线性关系,测定下限(10S/N)在1.0~2.5 μg·kg-1之间。加标回收率在91.0%~98.3%之间,测定值的相对标准偏差(n=6)在0.94%~2.7%之间。
Abstract
The sample (1.000 0 g) was added into the accelerated solvent extraction tank, then 10 mL of 5 mol·L-1 hydrochloric acid solution, 1 mL of 5 mol·L-1 potassium chloride solution and 2 mL of 10 mol·L-1 cysteine solution were added. The mixture was preheated at 8.0 MPa and 70℃ for 2 min, heated for 5 min, extracted statically for 5 min, and seperated. After repeating extraction twice, the extract was combined. Then 0.2 mL of 0.5 mol·L-1 cysteine solution and 1.5 mL of 6 mol·L-1 sodium hydroxide solution were added into the extract, and the mixture was centrifuged at 10 000 r·min-1 for 5 min. The supernatant was concentrated by nitrogen-blowing and the residue was diluted to 1 mL with nitric acid (5+95) solution. After filtration with 0.45 μm nylon membrane, methylmercury, ethylmercury, inorganic mercury, thiomersal and phenylmercury in the solution were separated on an Eclipse XDB-C18 reversed-phase column (150 mm×4.6 mm, 5.0 μm), with a mixture of 50 g·L-1 acetonitrile solution, 5 g·L-1 ammonium acetate solution and 1 g·L-1 cysteine solution (1:1:1, volume ratio) as the mobile phase, and determined by atomic fluorescence spectrometry. Linear relationships were found between the fluorescence intensity and mass concentraion of the five kinds of mercury species in definite ranges, with lower limits of determination (10S/N) in the range of 1.0-2.5 μg·kg-1. Values of recovery obtained by standard addition method ranged from 91.0% to 98.3%, and RSDs (n=6) ranged from 0.94% to 2.7%.
中图分类号 O657.3 DOI 10.11973/lhjy-hx201806015
所属栏目 工作简报
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收稿日期 2017/7/11
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备注陈德泉,工程师,研究方向为食品药品成分检测,65475366@qq.com
引用该论文: CHEN Dequan,LI Yan,YE Zebo. Determination of Five Kinds of Mercury Species in Shrimp Feed by LC-AFS with Accelerated Solvent Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(6): 698~702
陈德泉,李岩,叶泽波. 加速溶剂提取-液相色谱-原子荧光光谱法测定对虾饲料中5种形态的汞[J]. 理化检验-化学分册, 2018, 54(6): 698~702
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【3】杨桂朋,张启华.水环境及水产品中汞的测定与形态分析进展[J].中国海洋大学学报(自然科学版), 2011,41(11):67-80.
【4】HOFFMANN G G, BROCKNER W, STEINFATT I. Bis(n-alkanethiolato) mercury(Ⅱ) compounds, Hg(SC<i>nH2n+1)2 (n=1 to 10, 12):Preparation methods, vibrational spectra, GC/MS investigations, and exchange reactions with diorganyl disulfides[J]. Inorganic Chemistry, 2017,40(5):977-985.
【5】肖亚兵,秦德元,王伟,等.LC-AFS法对动物源性食品中硫柳汞残留量的测定[J].分析测试学报, 2011,30(6):661-664.
【6】LIU Z, XING Z, LI Z, et al. The online coupling of high performance liquid chromatography with atomic fluorescence spectrometry based on dielectric barrier discharge induced chemical vapor generation for the speciation of mercury[J]. Journal of Analytical Atomic Spectrometry, 2017,32(3):678-685.
【7】王媛,张宏斌,陆巧荣,等.微波辅助-液相色谱-原子荧光光谱法对水产品中汞的形态分析[J].中国卫生检验杂志, 2016,26(21):3101-3104.
【8】曾云想,梁婷婷,汤明河,等.液相色谱-原子荧光光谱法测定水产品中汞形态的含量[J].理化检验-化学分册, 2017,53(10):1226-1228.
【9】BROMBACH C C, GAJDOSECHOVA Z, CHEN B, et al. Direct online HPLC-CV-AFS method for traces of methylmercury without derivatisation:A matrix-independent method for urine, sediment and biological tissue samples[J]. Analytical and Bioanalytical Chemistry, 2015,407(3):973-981.
【10】SANCHEZRODAS D, MELLANO F, MORALES E, et al. A simplified method for inorganic selenium and selenoaminoacids speciation based on HPLC-TR-HG-AFS[J]. Talanta, 2013,106:298-304.
【11】ZENG X, SU S, FENG Q, et al. Arsenic speciation transformation and arsenite influx and efflux across the cell membrane of fungi investigated using HPLC-HG-AFS and in-situ XANES[J]. Chemosphere, 2015,119:1163-1168.
【12】彭国俊,朱晓艳,陈建国,等.高效液相色谱-电感耦合等离子体质谱联用快速测定水样和生物样品中的4种汞形态[J].分析试验室, 2015,34(1):44-48.
【13】贾彦博,陆吉琛,朱蓓,等.高效液相色谱-电感耦合等离子体质谱联用法测定东海乌参样品中的二价汞、甲基汞、乙基汞和苯基汞[J].食品安全质量检测学报, 2016,7(11):4609-4613.
【14】王萌,丰伟悦,张芳,等.高效液相色谱-电感耦合等离子体质谱联用测定生物样品中无机汞和甲基汞[J].分析化学, 2005,33(12):1671-1675.
【15】杭婧,冯晓青,胡晓抒.高效液相色谱-电感耦合等离子体质谱联用测定动物源性中药材中无机汞和甲基汞[J].分析仪器, 2016,48(6):89-94.
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