An Automatic Solid Phase Extraction and Ultra-Performance Liquid Chromatography Tandem Mass Spectrometry for Determination of Seven Microcystins at Ultra-Trace Levels in Surface Water
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摘要
A method was developed for the detection of seven microcystins(microcystin-LR, RR, YR, LA, LY, LW and LF) in surface water using automatic solid-phase extraction(A-SPE) coupled with ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). The automated solid-phase extraction system was used to extract microcystins(MCs) from water samples. UPLC-MS/MS was used to determine MCs concentrations in just 5 min. Method detection limits were from 0.3 to 0.9 ng/L, microcystin recoveries ranged from 83.8% to 114%, and the relative standard deviation(RSD) varied from 5.6% to 12.5%. This analytical approach was found to be simple, highly sensitive, accurate, which required little manual operation. Additionally, to validate this analytical method, A-SPE+UPLC-MS/MS was applied to characterize the concentration of MCs in Taihu Lake, Wuxi, China.
A method was developed for the detection of seven microcystins(microcystin-LR, RR, YR, LA, LY, LW and LF) in surface water using automatic solid-phase extraction(A-SPE) coupled with ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). The automated solid-phase extraction system was used to extract microcystins(MCs) from water samples. UPLC-MS/MS was used to determine MCs concentrations in just 5 min. Method detection limits were from 0.3 to 0.9 ng/L, microcystin recoveries ranged from 83.8% to 114%, and the relative standard deviation(RSD) varied from 5.6% to 12.5%. This analytical approach was found to be simple, highly sensitive, accurate, which required little manual operation. Additionally, to validate this analytical method, A-SPE+UPLC-MS/MS was applied to characterize the concentration of MCs in Taihu Lake, Wuxi, China.
A method was developed for the detection of seven microcystins(microcystin-LR, RR, YR, LA, LY, LW and LF) in surface water using automatic solid-phase extraction(A-SPE) coupled with ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). The automated solid-phase extraction system was used to extract microcystins(MCs) from water samples. UPLC-MS/MS was used to determine MCs concentrations in just 5 min. Method detection limits were from 0.3 to 0.9 ng/L, microcystin recoveries ranged from 83.8% to 114%, and the relative standard deviation(RSD) varied from 5.6% to 12.5%. This analytical approach was found to be simple, highly sensitive, accurate, which required little manual operation. Additionally, to validate this analytical method, A-SPE+UPLC-MS/MS was applied to characterize the concentration of MCs in Taihu Lake, Wuxi, China.
引文
[1]Dai R, Wang P, Jia P, et al. A review on factors affecting microcystins production by algae in aquatic environments[J].World Journal of Microbiology&Biotechnology, 2016,32(3):5.
[2]Hernandez J M, Lopez-Rodas V, Costas E. Microcystins from tap water could be a risk factor for liver and colorectal cancer:a risk intensified by global change[J]. Medical Hypotheses, 2009, 72(5):539-540.
[3]Zhang D W, Liao Q G, Zhang L, et al. Occurrence and spatial distributions of microcystins in Poyang Lake, the largest freshwater lake in China[J]. Ecotoxicology, 2015,24(1):19-28.
[4]Pekar H, Westerberg E, Bruno O, et al. Fast, rugged and sensitive ultra high pressure liquid chromatography tandem mass spectrometry method for analysis of cyanotoxins in raw water and drinking water-first findings of anatoxins,cylindrospermopsins and microcystin variants in Swedish source waters and infiltration ponds[J]. Journal of Chromatography A, 2016,1429:265-276.
[5]Munoz G, Voduy S, Roy-Lachapelle A, et al. Analysis of individual and total microcystins in surface water by on-line preconcentration and desalting coupled to liquid chromatography tandem mass spectrometry[J]. Journal of Chromatography A, 2017,1516:9-20.
[6]Rodrigues M A, Reis M P, Mateus M C. Liquid chromatography/negative electrospray ionization ion trap MS2 mass spectrometry application for the determination of microcystins occurrence in Southern Portugal water reservoirs[J]. Toxicon, 2013, 74:8-18.
[7]Steffen M M,Davis T W, Mckay R M, et al.Ecophysiological examination of the Lake Erie microcystis bloom in 2014:Linkages between biology and the water supply shutdown of Toledo, Ohio[J]. Environmental Science&Technology, 2017, 51(12):6745-6755.
[8]World Health Organization. Guidelines for Drinking-Water Quality[M]. 4th Edition. Geneva:WHO Press, 2011.
[9]Carmichael W W,An J. Using an enzyme linked immunosorbent assay(ELISA)and a protein phosphatase inhibition assay(PPIA)for the detection of microcystins and nodularins[J]. Natural Toxins. 1999, 7(6):377-385.
[10]Weller M G. Immunoassays and biosensors for the detection of cyanobacterial toxins in water[J]. Sensors, 2013, 13(11):15085-15112.
[11]Beltran E, Ibanez M, Sancho J V, et al. Determination of six microcystins and nodularin in surface and drinking waters by on-line solid phase extraction-ultra high pressure liquid chromatography tandem mass spectrometry[J]. Journal of Chromatography A, 2012, 1266(10):61-68.
[12]Shen F,Wang L H,Zhou Q, et al. Simultaneous determination of aniline, benzidine,microcystins, and carbaryl in water using ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry[J].Water, Air,&Soil Pollution, 2017, 228(2):69.
[13]Herry S E, Fathalli A, Rejeb J B, et al. Seasonal occurrence and toxicity of Microcystis spp. and Oscillatoria tenuis in the Lebna Dam, Tunisia[J]. Water Research, 2008, 42(4):1263-1273.
[14]Kim E M, Lee J S, Choi S K, et al. Analysis of ketamine and norketamine in urine by automatic solid-phase extraction(SPE)and positive ion chemical ionization-gas chromatography-mass spectrometry(PCI-GC-MS)[J].Forensic Science International, 2008, 174(2-3):197-202.
[15]Rhee J, Cho B, Lee J, et al. Liquid chromatography with tandem mass spectrometry for the determination of flufenoxuron in blood using automatic solid phase extraction and its application to a fatal case of flufenoxuron poisoning[J]. Forensic Science International, 2015, 257:49-53.
[16]Parsekian A D, Regnery J, Wing A D, et al. Geophysical and hydrochemical identification of flow paths with implications for water quality at an ARR site[J]. Groundwater Monitoring&Remediation, 2014, 34(3):105-116.
[17]Colume A,Cardenas S,Mercedes Gallego A, et al.Multiresidue screening of pesticides in fruits using an automatic solid-phase extraction system[J]. Journal of Agricultural&Food Chemistry, 2001, 49(3):1109-1116.
[18]Maizels M, Budde W L. A LC/MS method for the determination of cyanobacteria toxins in water[J].Analytical Chemistry, 2004, 76(5):1342-1351.
[19]Shen F,Xu Y J,Jiang S, et al. Determination of microcystins in algal bloom samples by ultra performance liquid chromatography-tandem mass spectrometry and elimination of their matrix effects[J]. Chinese Journal of Chromatography, 2017, 35(7):772-777(Ch).
[20]Barco M, Lawton L A, Rivera J, et al. Optimization of intracellular microcystin extraction for their subsequent analysis by high-performance liquid chromatography[J].Journal of Chromatography A, 2005, 1074(1):23-30.
[21]Zhang M, Tang F, Chen F, et al. Simultaneous determination of nine microcystins in surface water by solid phase extraction and ultra performance liquid chromatographyelectrospray ionization tandem mass spectrometry[J].Chinese Journal of Chromatography, 2012, 30(1):51-55(Ch).
[22]Rogers S, Puddick J, Wood S A, et al. The effect ofcyanobacterial biomass enrichment by centrifugation and GF/C filtration on subsequent microcystin measurement[J].Toxins, 2015, 7(3):821-834.
[23]United States Environmental Protection Agency. U.S. Code of Federal Regulations; Guidelines Establishing Test Procedures for the Analysis of Pollutants-Appendix B[M].Washington D C:United States Government Printing Office,1999.
[24]United States Environmental Protection Agency. Determination of Microcystins and Nodularin in Drinking Water by Solid Phase Extraction and Liquid Chromatogra-phy/Tandem Mass Spectrometry(LC/MS/MS)[M]. Washington D C:United States Government Printing Office, 2015.
[2]Hernandez J M, Lopez-Rodas V, Costas E. Microcystins from tap water could be a risk factor for liver and colorectal cancer:a risk intensified by global change[J]. Medical Hypotheses, 2009, 72(5):539-540.
[3]Zhang D W, Liao Q G, Zhang L, et al. Occurrence and spatial distributions of microcystins in Poyang Lake, the largest freshwater lake in China[J]. Ecotoxicology, 2015,24(1):19-28.
[4]Pekar H, Westerberg E, Bruno O, et al. Fast, rugged and sensitive ultra high pressure liquid chromatography tandem mass spectrometry method for analysis of cyanotoxins in raw water and drinking water-first findings of anatoxins,cylindrospermopsins and microcystin variants in Swedish source waters and infiltration ponds[J]. Journal of Chromatography A, 2016,1429:265-276.
[5]Munoz G, Voduy S, Roy-Lachapelle A, et al. Analysis of individual and total microcystins in surface water by on-line preconcentration and desalting coupled to liquid chromatography tandem mass spectrometry[J]. Journal of Chromatography A, 2017,1516:9-20.
[6]Rodrigues M A, Reis M P, Mateus M C. Liquid chromatography/negative electrospray ionization ion trap MS2 mass spectrometry application for the determination of microcystins occurrence in Southern Portugal water reservoirs[J]. Toxicon, 2013, 74:8-18.
[7]Steffen M M,Davis T W, Mckay R M, et al.Ecophysiological examination of the Lake Erie microcystis bloom in 2014:Linkages between biology and the water supply shutdown of Toledo, Ohio[J]. Environmental Science&Technology, 2017, 51(12):6745-6755.
[8]World Health Organization. Guidelines for Drinking-Water Quality[M]. 4th Edition. Geneva:WHO Press, 2011.
[9]Carmichael W W,An J. Using an enzyme linked immunosorbent assay(ELISA)and a protein phosphatase inhibition assay(PPIA)for the detection of microcystins and nodularins[J]. Natural Toxins. 1999, 7(6):377-385.
[10]Weller M G. Immunoassays and biosensors for the detection of cyanobacterial toxins in water[J]. Sensors, 2013, 13(11):15085-15112.
[11]Beltran E, Ibanez M, Sancho J V, et al. Determination of six microcystins and nodularin in surface and drinking waters by on-line solid phase extraction-ultra high pressure liquid chromatography tandem mass spectrometry[J]. Journal of Chromatography A, 2012, 1266(10):61-68.
[12]Shen F,Wang L H,Zhou Q, et al. Simultaneous determination of aniline, benzidine,microcystins, and carbaryl in water using ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry[J].Water, Air,&Soil Pollution, 2017, 228(2):69.
[13]Herry S E, Fathalli A, Rejeb J B, et al. Seasonal occurrence and toxicity of Microcystis spp. and Oscillatoria tenuis in the Lebna Dam, Tunisia[J]. Water Research, 2008, 42(4):1263-1273.
[14]Kim E M, Lee J S, Choi S K, et al. Analysis of ketamine and norketamine in urine by automatic solid-phase extraction(SPE)and positive ion chemical ionization-gas chromatography-mass spectrometry(PCI-GC-MS)[J].Forensic Science International, 2008, 174(2-3):197-202.
[15]Rhee J, Cho B, Lee J, et al. Liquid chromatography with tandem mass spectrometry for the determination of flufenoxuron in blood using automatic solid phase extraction and its application to a fatal case of flufenoxuron poisoning[J]. Forensic Science International, 2015, 257:49-53.
[16]Parsekian A D, Regnery J, Wing A D, et al. Geophysical and hydrochemical identification of flow paths with implications for water quality at an ARR site[J]. Groundwater Monitoring&Remediation, 2014, 34(3):105-116.
[17]Colume A,Cardenas S,Mercedes Gallego A, et al.Multiresidue screening of pesticides in fruits using an automatic solid-phase extraction system[J]. Journal of Agricultural&Food Chemistry, 2001, 49(3):1109-1116.
[18]Maizels M, Budde W L. A LC/MS method for the determination of cyanobacteria toxins in water[J].Analytical Chemistry, 2004, 76(5):1342-1351.
[19]Shen F,Xu Y J,Jiang S, et al. Determination of microcystins in algal bloom samples by ultra performance liquid chromatography-tandem mass spectrometry and elimination of their matrix effects[J]. Chinese Journal of Chromatography, 2017, 35(7):772-777(Ch).
[20]Barco M, Lawton L A, Rivera J, et al. Optimization of intracellular microcystin extraction for their subsequent analysis by high-performance liquid chromatography[J].Journal of Chromatography A, 2005, 1074(1):23-30.
[21]Zhang M, Tang F, Chen F, et al. Simultaneous determination of nine microcystins in surface water by solid phase extraction and ultra performance liquid chromatographyelectrospray ionization tandem mass spectrometry[J].Chinese Journal of Chromatography, 2012, 30(1):51-55(Ch).
[22]Rogers S, Puddick J, Wood S A, et al. The effect ofcyanobacterial biomass enrichment by centrifugation and GF/C filtration on subsequent microcystin measurement[J].Toxins, 2015, 7(3):821-834.
[23]United States Environmental Protection Agency. U.S. Code of Federal Regulations; Guidelines Establishing Test Procedures for the Analysis of Pollutants-Appendix B[M].Washington D C:United States Government Printing Office,1999.
[24]United States Environmental Protection Agency. Determination of Microcystins and Nodularin in Drinking Water by Solid Phase Extraction and Liquid Chromatogra-phy/Tandem Mass Spectrometry(LC/MS/MS)[M]. Washington D C:United States Government Printing Office, 2015.