应用ICP-MS/MS快速测定红酒中的多种微量元素
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摘要
建立电感耦合等离子体-串联质谱法测定红酒中多元素的分析方法。采用0.45μm的纤维滤膜对红酒进行过滤后经硝酸酸化直接进样分析。通过优化仪器的工作参数,在串联质谱模式下,采用不同反应气通过质量转移反应消除质谱干扰,各元素的检出限在1.4～51.8 ng/L范围内,样品的加标回收率在94.0%～104.7%之间,相对标准偏差不大于4.0%。方法具有简单快速、检出限低、准确性好和精密度高的特点,适用于红酒中多元素的检测。
An analytical method using inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) was established for determining multi-elements (Cr, Mn, Fe, Ni, Cu, Zn, As, Se, Cd, Sn, Hg and Pb) in red wine. Samples were filtered through a 0.45 μm pore size cellulose filter, and after acidification with nitric acid, the filtrate was directly analyzed. Instrumental parameters were optimized so that elimination of inferences was achieved via mass-shift reaction of different reaction gases. The limits of detection (LOD) were in the range of 1.4–51.8 ng/L for all analytes. The recoveries for spiked samples were in the range of 94.0%–104.7%, with relative standard deviations (RSDs) no more than 4.0%. The method is simple and fast with low detection limit, good accuracy and high precision, making it suitable for the determination of multielements in red wine.
An analytical method using inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) was established for determining multi-elements (Cr, Mn, Fe, Ni, Cu, Zn, As, Se, Cd, Sn, Hg and Pb) in red wine. Samples were filtered through a 0.45 μm pore size cellulose filter, and after acidification with nitric acid, the filtrate was directly analyzed. Instrumental parameters were optimized so that elimination of inferences was achieved via mass-shift reaction of different reaction gases. The limits of detection (LOD) were in the range of 1.4–51.8 ng/L for all analytes. The recoveries for spiked samples were in the range of 94.0%–104.7%, with relative standard deviations (RSDs) no more than 4.0%. The method is simple and fast with low detection limit, good accuracy and high precision, making it suitable for the determination of multielements in red wine.
引文
[1]连晓文,杨秀环,梁旭霞.ICP-MS法快速测定葡萄酒中11种微量元素[J].中国卫生检验杂志,2005,15(8):925-927.DOI:10.3969/j.issn.1004-8685.2005.08.011.
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[20]DRONOV M,KOZA T,SCHWIERS A,et al.Strontium carbonate precipitation as a sample preparation technique for isotope ratio analysis of Sr in mineral water and wine by quadrupolebased inductively coupled plasma mass spectrometry[J].Rapid Communications in Mass Spectrometry,2018,32(2):149-158.DOI:10.1002/rcm.8018.
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[22]LAO M,COMPANYS E,WENG L,et al.Speciation of Zn,Fe,Ca and Mg in wine with the Donnan membrane technique[J].Food Chemistry,2018,239:1143-1150.DOI:10.1016/j.foodchem.2017.07.040.
[23]MIN S C,RYU J S,PARK H Y,et al.Precise determination of the lithium isotope ratio in geological samples using MC-ICP-MS with cool plasma[J].Journal of Analytical Atomic Spectrometry,2013,28(4):505-509.DOI:10.1039/C2JA30293D.
[24]BARELA P S,SILVA N A,PEREIRA J S F,et al.Microwaveassisted digestion using diluted nitric acid for further trace elements determination in biodiesel by SF-ICP-MS[J].Fuel,2017,204:85-90.DOI:10.1016/j.fuel.2017.05.028.
[25]WU D,PICHLER T.Simultaneous speciation analysis of As,Sb and Se redox couples by SF-ICP-MS coupled to HPLC[J].Analytical Methods,2014,6(14):5112-5119.DOI:10.1039/C4AY01013B.
[26]BOLEA-FEMANDEZ E,BALCAEN L,RESANO M,et al.Overcoming spectral overlap via inductively coupled plasma-tandem mass spectrometry (ICP MS/MS).A tutorial review[J].Journal of Analytical Atomic Spectrometry,2017,32:1660-1679.DOI:10.1039/c7ja00010c.
[27]HE Q,XING Z,WEI C,et al.Rapid screening of copper intermediates in Cu(I)-catalyzed azide-alkyne cycloaddition using a modified ICP-MS/MS platform[J].Chemical Communications,2016,52(69):10501-10504.DOI:10.1039/c6cc04793a.
[28]DEITRICH C L,CUELLO-NUNEZ S,KMIOTEK D,et al.Accurate quantification of selenoprotein P(SEPP1) in plasma using isotopically enriched seleno-peptides and species-specific isotope dilution with HPLC coupled to ICP-MS/MS[J].Analytical Chemistry,2016,88(12):6357-6365.DOI:10.1021/acs.analchem.6b00715.
[29]WALKNER C,GRATZER R,MEISEL T,et al.Multi-element analysis of crude oils using ICP-QQQ-MS[J].Organic Geochemistry,2017,103:22-30.DOI:10.1016/j.orggeochem.2016.10.009.
[30]BOLEA-FEMANDEZ E,PHAN K,BALCAEN L,et al.Determination of ultra-trace amounts of prosthesis-related metals in whole blood using volumetric absorptive micro-sampling and tandem ICP-mass spectrometry[J].Analytica Chimica Acta,2016,941:1-9.DOI:10.1016/j.aca.2016.08.030.
[2]杜建中,陈婷,刘木球,等.红酒中添加红色素的快速检测[J].食品科学,2014,35(10):200-206.DOI:10.7506/spkx1002-6630-201410038.
[3]胡力川,黄海霞.火焰原子吸收光谱法测定红酒中微量元素的含量[J].微量元素与健康研究,2014,31(3):34-35.DOI:10.3969/j.issn.1002-3127.2003.03.007.
[4]张云峰,李艳,严斌,等.葡萄园土壤中铜、铁、锌、锰四种金属元素的分析与研究[J].食品科学,2010,31(24):374-379.DOI:10.7506/spkx1002-6630-201024082.
[5]杨晨露,王华,李华.中/欧葡萄酒工艺标准比较[J].食品与发酵工业,2017,43(2):252-257.DOI:10.13995/j.cnki.11-1802/ts.201702043.
[6]CASTINEIRA M M,BRANDT R,VON BOHLEN A,et al.Development of a procedure for the multi-element determination of trace elements in wine by ICP-MS[J].Fresenius’Journal of Analytical Chemistry,2001,370(5):553-558.DOI:10.1007/s002160100862.
[7]VIAN M A,TOMAO V,GALLET S,et al.Simple and rapid method for cis-and trans-resveratrol and piceid isomers determination in wine by high-performance liquid chromatography using Chromolith columns[J].Journal of Chromatography A,2005,1085(2):224-229.DOI:10.1016/j.chroma.2005.05.083.
[8]LV Z,YOU J,LU S,et al.Sensitive determination of thiols in wine samples by a stable isotope-coded derivatization reagent d0/d4-acridone-10-ethyl-N-maleimide coupled with high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry analysis[J].Journal of Chromatography A,2017,1491:98-107.DOI:10.1016/j.chroma.2017.02.042.
[9]FONTANA A R,BOTTINI R.Filter-vial dispersive solid-phase extraction as a simplified clean-up for determination of ethylphenols in red wines[J].Food Chemistry,2017,230:405-410.DOI:10.1016/j.foodchem.2017.03.084.
[10]BARCIELA-ALONSO M,OTERO-LAVANDEIRA N,BERMEJO-BARRERA P.Solid phase extraction using molecular imprinted polymers for phthalate determination in water and wine samples by HPLC-ESI-MS[J].Microchemical Journal,2017,132:233-237.DOI:10.1016/j.microc.2017.02.007.
[11]ACETO M,ABOLLINO O,BRUZZONITI M C,et al.Determination of metals in wine with atomic spectroscopy (flame-AAS,GF-AAS and ICP-AES);a review[J].Food Additives&Contaminants,2002,19(2):126-133.DOI:10.1080/02652030110071336.
[12]FRESCHI G P G,DAKUZAKU C S,MORAES M,et al.Simultaneous determination of cadmium and lead in wine by electrothermal atomic absorption spectrometry[J].Spectrochimica Acta Part B:Atomic Spectroscopy,2001,56(10):1987-1993.DOI:10.1016/S0584-8547(01)00331-7.
[13]MOLLO A,SIXTO A,FALCHI L,et al.Zinc determination in Tannat wine by direct injection onto graphite tube:electrothermal AAS as an alternative to flame AAS[J].Microchemical Journal,2017,135:239-244.DOI:10.1016/j.microc.2017.09.008.
[14]SELIH V S,SALA M,DRGAN V.Multi-element analysis of wines by ICP-MS and ICP-OES and their classification according to geographical origin in Slovenia[J].Food Chemistry,2014,153:414-423.DOI:10.1016/j.foodchem.2013.12.081.
[15]PANEQUE P,MORALES M L,BURGOS P,et al.Elemental characterisation of Andalusian wine vinegars with protected designation of origin by ICP-OES and chemometric approach[J].Food Control,2016,75:203-210.DOI:10.1016/j.foodcont.2016.12.006.
[16]OZBEK N,AKMAN S.Determination of boron in Turkish wines by microwave plasma atomic emission spectrometry[J].LWT-Food Science and Technology,2015,61(2):532-535.DOI:10.1016/j.lwt.2014.11.047.
[17]COETZEE P P,VAN JAARSVELD F P,VANHAECKE F.Intraregional classification of wine via ICP-MS elemental fingerprinting[J].Food Chemistry,2014,164:485-492.DOI:10.1016/j.foodchem.2014.05.027.
[18]WANG X,LIU J,WANG X,et al.Direct quantification of total sulfur dioxide in wine using triple quadrupole ICP-MS[J].Analytical Methods,2015,7:3224-3228.DOI:10.1039/C4AY02863E.
[19]COETZEE P P,STEFFENS F E,EISELEN R J,et al.Multi-element analysis of south African wines by ICP-MS and their classification according to geographical origin[J].Journal of Agricultural&Food Chemistry,2005,53(13):5060-5066.DOI:10.1021/jf048268n.
[20]DRONOV M,KOZA T,SCHWIERS A,et al.Strontium carbonate precipitation as a sample preparation technique for isotope ratio analysis of Sr in mineral water and wine by quadrupolebased inductively coupled plasma mass spectrometry[J].Rapid Communications in Mass Spectrometry,2018,32(2):149-158.DOI:10.1002/rcm.8018.
[21]芮玉奎,于庆泉,金银花,等.应用ICP-MS快速测定葡萄酒中40种元素的含量[J].光谱学与光谱分析,2007,27(5):1015-1017.DOI:10.3321/j.issn:1000-0593.2007.05.045.
[22]LAO M,COMPANYS E,WENG L,et al.Speciation of Zn,Fe,Ca and Mg in wine with the Donnan membrane technique[J].Food Chemistry,2018,239:1143-1150.DOI:10.1016/j.foodchem.2017.07.040.
[23]MIN S C,RYU J S,PARK H Y,et al.Precise determination of the lithium isotope ratio in geological samples using MC-ICP-MS with cool plasma[J].Journal of Analytical Atomic Spectrometry,2013,28(4):505-509.DOI:10.1039/C2JA30293D.
[24]BARELA P S,SILVA N A,PEREIRA J S F,et al.Microwaveassisted digestion using diluted nitric acid for further trace elements determination in biodiesel by SF-ICP-MS[J].Fuel,2017,204:85-90.DOI:10.1016/j.fuel.2017.05.028.
[25]WU D,PICHLER T.Simultaneous speciation analysis of As,Sb and Se redox couples by SF-ICP-MS coupled to HPLC[J].Analytical Methods,2014,6(14):5112-5119.DOI:10.1039/C4AY01013B.
[26]BOLEA-FEMANDEZ E,BALCAEN L,RESANO M,et al.Overcoming spectral overlap via inductively coupled plasma-tandem mass spectrometry (ICP MS/MS).A tutorial review[J].Journal of Analytical Atomic Spectrometry,2017,32:1660-1679.DOI:10.1039/c7ja00010c.
[27]HE Q,XING Z,WEI C,et al.Rapid screening of copper intermediates in Cu(I)-catalyzed azide-alkyne cycloaddition using a modified ICP-MS/MS platform[J].Chemical Communications,2016,52(69):10501-10504.DOI:10.1039/c6cc04793a.
[28]DEITRICH C L,CUELLO-NUNEZ S,KMIOTEK D,et al.Accurate quantification of selenoprotein P(SEPP1) in plasma using isotopically enriched seleno-peptides and species-specific isotope dilution with HPLC coupled to ICP-MS/MS[J].Analytical Chemistry,2016,88(12):6357-6365.DOI:10.1021/acs.analchem.6b00715.
[29]WALKNER C,GRATZER R,MEISEL T,et al.Multi-element analysis of crude oils using ICP-QQQ-MS[J].Organic Geochemistry,2017,103:22-30.DOI:10.1016/j.orggeochem.2016.10.009.
[30]BOLEA-FEMANDEZ E,PHAN K,BALCAEN L,et al.Determination of ultra-trace amounts of prosthesis-related metals in whole blood using volumetric absorptive micro-sampling and tandem ICP-mass spectrometry[J].Analytica Chimica Acta,2016,941:1-9.DOI:10.1016/j.aca.2016.08.030.