液相色谱-串联质谱法测定蜂王浆中新型烟碱类药物及其代谢物残留量
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摘要
采用QuEChERS净化-液相色谱-串联质谱法(QuEChERS-LC-MS/MS)测定蜂王浆中新型烟碱类药物吡蚜酮、呋虫胺、烯啶虫胺、噻虫嗪、氟啶虫酰胺及代谢物4-(三氟甲基)烟酰胺、吡虫啉、噻虫胺、氯噻啉、啶虫脒及代谢物N-去甲基啶虫脒和噻虫啉的残留量。样品经水稀释,甲醇沉淀蛋白并提取,以N-丙基乙二胺(PSA)、C18和无水硫酸镁作为分散剂进行QuEChERS净化,采用液相色谱-串联质谱法进行检测(电喷雾离子源,正离子模式,多反应监测模式),以同位素内标法和外标法进行定量分析。结果表明,该方法定量限以S/N=10计,吡呀酮、呋虫胺为2.5μg/kg,烯啶虫胺、氯噻啉、啶虫脒、噻虫啉为5.0μg/kg,噻虫嗪、氟啶虫酰胺、吡虫啉、噻虫胺、4-(三氟甲基)烟酰胺、N-去甲基啶虫脒为12.5μg/kg。线性相关系数大于0.996。对空白蜂王浆进行添加回收实验,回收率为81.2%～119%;相对标准偏差为1.7%～12.2%。该方法简便、快捷,定量限能够满足目前国内外最大残留限量的要求,可作为蜂王浆中新型烟碱类药物及其代谢物残留量的测定方法。
Pymetrozine, dinotefuran, nitenpyram, thiamethoxam, flonicamid and its metabolite(4-trifluoromethylnicotinamide), imidacloprid, clothianidin, imidaclothiz, acetamiprid and its metabolite(N-desmethylacetamiprid)) and thiacloprid residues in royal-jelly were detected by QuEChERS-LC-MS/MS. The royal-jelly samples were diluted by water, the protein of royal-jelly was precipitated by methanol and then the methanol supernatant solution was cleaned up with PSA, C18 and MgSO_4 by QuEChERS method, the supernatant solution was evaporated to dryness and reconstituted in methanol-0.15% formic acid solution(1∶9, V/V), and then filtered through nylon membrane into a glass LC vial for LC-MS/MS analysis. The solution was separated by Agilent Eclipse XDB-C18 column(150 mm×4.6 mm×5 μm) and the quantitative detection was performed on LC-MS/MS by multiple reaction monitoring(MRM) mode under positive electrospray ionization mode(ESI~+). Isotopes internal standard method(dinotefuran, thiamethoxam, imidacloprid, clothianidin, acetamiprid and thiacloprid) and external standard method(pymetrozine, nitenpyram, flonicamid, 4-trifluoromethylnicotinamide, imidaclothiz and N-desmethylacetamiprid) were used for quantitation analysis. The limits of quantification(LOQs, S/N=10) of pymetrozine, dinotefuran are 2.5 μg/kg, nitenpyram, imidaclothiz, acetamiprid, thiacloprid are 5.0 μg/kg, thiamethoxam, flonicamid, imidacloprid, clothianidin, 4-trifluoromethylnicotinamide, N-desmethylacetamiprid are 12.5 μg/kg, respectively. The correlation coefficients are more than 0.996, the recoveries and the relative standard deviations(RSD) are 81.2%-119% and 1.7%-12.2%, respectively. This method is convenient, rapid and effective, QuEChERS(quick, easy, cheap, effective and rugged) is suitable for determination and confirmation of pymetrozine, dinotefuran, nitenpyram, thiamethoxam, flonicamid and its metabolite(4-trifluoromethylnicotinamide), imidacloprid, clothianidin, imidaclothiz, thiacloprid, acetamiprid and its metabolite(N-desmethylacetamiprid).
Pymetrozine, dinotefuran, nitenpyram, thiamethoxam, flonicamid and its metabolite(4-trifluoromethylnicotinamide), imidacloprid, clothianidin, imidaclothiz, acetamiprid and its metabolite(N-desmethylacetamiprid)) and thiacloprid residues in royal-jelly were detected by QuEChERS-LC-MS/MS. The royal-jelly samples were diluted by water, the protein of royal-jelly was precipitated by methanol and then the methanol supernatant solution was cleaned up with PSA, C18 and MgSO_4 by QuEChERS method, the supernatant solution was evaporated to dryness and reconstituted in methanol-0.15% formic acid solution(1∶9, V/V), and then filtered through nylon membrane into a glass LC vial for LC-MS/MS analysis. The solution was separated by Agilent Eclipse XDB-C18 column(150 mm×4.6 mm×5 μm) and the quantitative detection was performed on LC-MS/MS by multiple reaction monitoring(MRM) mode under positive electrospray ionization mode(ESI~+). Isotopes internal standard method(dinotefuran, thiamethoxam, imidacloprid, clothianidin, acetamiprid and thiacloprid) and external standard method(pymetrozine, nitenpyram, flonicamid, 4-trifluoromethylnicotinamide, imidaclothiz and N-desmethylacetamiprid) were used for quantitation analysis. The limits of quantification(LOQs, S/N=10) of pymetrozine, dinotefuran are 2.5 μg/kg, nitenpyram, imidaclothiz, acetamiprid, thiacloprid are 5.0 μg/kg, thiamethoxam, flonicamid, imidacloprid, clothianidin, 4-trifluoromethylnicotinamide, N-desmethylacetamiprid are 12.5 μg/kg, respectively. The correlation coefficients are more than 0.996, the recoveries and the relative standard deviations(RSD) are 81.2%-119% and 1.7%-12.2%, respectively. This method is convenient, rapid and effective, QuEChERS(quick, easy, cheap, effective and rugged) is suitable for determination and confirmation of pymetrozine, dinotefuran, nitenpyram, thiamethoxam, flonicamid and its metabolite(4-trifluoromethylnicotinamide), imidacloprid, clothianidin, imidaclothiz, thiacloprid, acetamiprid and its metabolite(N-desmethylacetamiprid).
引文
[1] 刘喜生,李春雁,靳藜. 蜂王浆的药理和生理作用[J]. 中国蜂业,2015,66(5):48-49. LIU Xisheng, LI Chunyan, JIN Li.The pharmacological and physiological effects of royal jelly[J]. Apiculture of China, 2015, 66(5): 48-49(in Chinese).
[2] WU L M, CHEN L Z, SELVARAJ J N, WEI Y, WANG Y, LI Y, ZHAO J, XUE X F. Identification of the distribution of adenosine phosphates, nucleosides and nucleobases in royal jelly[J]. Food Chemistry, 2015, (173): 1 111-1 118.
[3] 中国医药保健品进出口商会. 2012年蜂王浆产品出口额创十年最高[J]. 中国蜂业,2013,(64):45-46. China Chamber of Commerce for Import & Export of Medicines & Health Products.In 2012,The highest level for export of royal jelly products in last ten years[J]. Apiculture of China, 2013, (64): 45-46(in Chinese).
[4] XU X, GAO Y X.Isolation and characterization of proteins and lipids from honeybee (Apismellifera L.) queen larvae and royal jelly[J]. Food Research International, 2013, 54(1): 330-337.
[5] PASTOR-BELDA M, GARRIDO I, CAMPILLO N, VI?AS P, HELLíN P, FLORES P, FENOLL J. Determination of spirocyclic tetronic/tetramic acid derivatives and neonicotinoid insecticides in fruits and vegetables by liquid chromatography and mass spectrometry after dispersive liquid-liquid microextraction[J]. Food Chemitry, 2016, (202): 389-395.
[6] CHAGNON M, KREUTZWEISER D, MITCHELL E A, MORRISSEY C A, NOOME D A, SLUIJS J P V. Risks of large scale use of systemic insecticides to ecosystem functioning and services[J]. Environmental Science and Pollution Research, 2012, 22(1): 119-134.
[7] LU C, WARCHOL K M, CALLAHAN R A. In situ replication of honey bee colony collapse disorder[J]. Bulletin of Insectology, 2012, 65(1): 99-106.
[8] LAURINO D, MANINO A, PATETTA A, PORPORATO M. Toxicity of neonicotinoid insecticides on different honey bee genotypes[J].Bulletin of Insectology, 2013, 66(1): 119-126.
[9] VICHAPONG J, BURAKHAM R, SRIJARANAI S. In-coupled syringe assisted octanol-water partition microextraction coupled with high-performance liquid chromatography for simultaneous determination of neonicotinoid insecticide residues in honey[J]. Talanta, 2015, (139): 21-26.
[10] MITCHELL E A D, MULHAUSER B, MULOT M, MUTABAZI A, GLAUSER G, AEBI A. A world wide survey of neonicotinoids in honey[J]. Science, 2017, 358(6 359): 109-111.
[11] The European Union. EU pesticides database[EB/OL]. https://ec.europa.eu/food/plant/pesticides/2018/05/01.
[12] Japan. Positive list system for agricultural chemical residues in foods[EB/OL]. http://www.mhlw.go.jp/english/topics/foodsafety/positivelist060228/2018/05/01.
[13] 许秀莹,施海燕,王鸣华. 气相色谱-质谱联用测定大米中种烟碱类农药残留[J]. 质谱学报,2012,33(2):99-103. XU Xiuying, SHI Haiyan, WANG Minghua.Determination of six neonicotinoid pesticides residue in rice by GC/MS[J]. Journal of Chinese Mass Spectrometry Society, 2012, 33(2): 99-103(in Chinese).
[14] GB/T 19648—2006 水果和蔬菜中500种农药及相关化学品残留量的测定气相色谱-质谱法[S]. 北京:中国标准出版社,2006.
[15] KO A Y, RAHMAN M M, ABD EL-ATY A M, JANG J, PARK J H, CHO S K, SHIM J H. Development of a simple extraction and oxidation procedure for the residue analysis of imidacloprid and its metabolites in lettuce using gas chromatography[J]. Food Chemistry, 2014, 148(3): 402-409.
[16] CAMPILLO N, VINAS P, FEREZ-MELGAREJO G, HERNANDEZ-CORDOBA M. Liquid chromatography with diode array detection and tandem mass spectrometry for the determination of neonicotinoid insecticides in honey samples using dispersive liquid-liquid microextraction[J]. Journal of Agricultural and Food Chemistry, 2013, (61): 4 799-4 805.
[17] 侯如燕,蔡荟梅,张正竹,宛晓春. 液相色谱法检测水果蔬菜中的烟碱类农药残留[J]. 分析试验室,2010,29(2):59-63. HOU Ruyan, CAI Huimei, ZHANG Zhengzhu, WAN Xiaochun.Determination of neonicotinoid pesticide residues in vegetables and fruits with high-performance liquid chromatography with diode-array detection[J]. Chinese Journal of Analysis Laboratory, 2010, 29(2): 59-63(in Chinese).
[18] 侯如燕,卞红正,赵秀霞,胡秭芳,苏婷,王孝辉,宛晓春. 固相萃取-液相色谱测定复杂基质蔬菜中 9种烟碱类残留[J]. 分析测试学报,2011,30(1):58-63. HOU Ruyan, BIAN Zhenghong, ZHAO Xiuxia, HU Zifang, SU Ting, WANG Xiaohui, WAN Xiaochun. Determination of nicotinoid residues in complicated matrix vegetables by solid phase extraction and HPLC method[J]. Journal of Instrumental Analysis, 2011, 30(1): 58-63(in Chinese).
[19] GARCíA M D, GALERA M M, VALVERDE R S, GALANTI A, GIROTTI S. Column switching liquid chromatography and post-column photochemically fluorescence detection to determine imidacloprid and 6-chloronicotinic acid in honeybees[J]. Journal of Chromatography A, 2007, (1 147): 17-23.
[20] RANCAN M, SABATINI A G, ACHILLI G, GALLETTI G C. Determination of imidacloprid and metabolites by liquid chromatography with an electrochemical detector and post column photochemical reactor[J]. Analytica Chimica Acta, 2006, 555(1): 20-24.
[21] 王东,侯传金,赵尔成,贾春虹. 盐析辅助均相液液萃取/分散固相萃取-超高效液相色谱串联质谱法测定蜂蜜中新烟碱类农药残留[J]. 分析测试学报,2015,34(6):681-685. WANG Dong, HOU Chuanjin, ZHAO Ercheng, JIA Chunhong.Determination of neonicotinoid residues in honey by ultra performance liquid chromatography-tandem mass spectrometry combined with salting-out homogeneous liquid-liquid extraction and dispersive solid-phase extraction[J]. Journal of Instrumental Analysis, 2015, 34(6): 681-685(in Chinese).
[22] 粟有志,李芳,齐鑫,史秀丽,王振宝. QuEChERS-高效液相色谱/串联质谱法同时测定蜂蜜中9种新烟碱类杀虫剂残留[J]. 分析科学学报,2015,31(2):203-207. SU Youzhi, LI Fang, QI Xin, SHI Xiuli, WANG Zhenbao. Determination of nine neonicotinoid insecticides in honey by QuEChERS-high performance liquid chromatography-tandem mass spectrometry[J]. Journal of Analytical Science, 2015, 31(2): 203-207(in Chinese).
[23] TANNER G, CZERWENKA C. LC-MS/MS Analysis of neonicotinoid insecticides in honey methodology and residue findings in Austrian honeys[J]. Journal of Agricultural and Food Chemistry, 2011, 59(23): 12 271-12 277.
[24] JIAO W T, XIAO Y, QIAN X S, TONG M M, HU Y Z, HOU R Y, HUA R M. Optimized combination of dilution and refined QuEChERS to overcome matrix effects of six types of tea for determination eight neonicotinoid insecticides by ultra performance liquid chromatograph-electrospray tandem mass spectrometry[J]. Food Chemistry, 2016, (210): 26-34.
[25] GBYLIK-SIKORSKA M, SNIEGOCKI T, POSYNIAK A. Determination of neonicotinoid insecticides and their metabolites in honey bee and honey by liquid chromatography tandem mass spectrometry[J]. Journal of Chromatography B, 2015, (990): 132-140.
[26] SUGANTHI A, BHUVANESWARI K, RAMYA M.Determination of neonicotinoid insecticide residues in sugarcane juice using LC-MS/MS[J]. Food Chemistry, 2018, (241): 275-280.
[27] GB/T 20769—2008 水果和蔬菜中450种农药及相关化学品残留量的测定液相色谱-串联质谱法[S]. 北京:中国标准出版社,2006.
[28] GB/T 23205—2008 茶叶中448种农药及相关化学品残留量的测定液相色谱-串联质谱法[S]. 北京:中国标准出版社,2008.
[29] VALVERDE S, ARES A M, ARRIBAS M, BERNAL J L, NOZAL M J. Development and validation of UHPLC-MS/MS methods for determination of neonicotinoid insecticides in royal jelly-based products[J]. Journal of Food Composition and Analysis, 2018, (70): 105-113.
[30] HOU J B, XIE W, HONG D, ZHANG W H, LI F, QIAN Y, HAN C. Simultaneous determination of ten neonicotinoid insecticides and two metabolites in honey and Royal-jelly by solid-phase extraction and liquid chromatography-tandem mass spectrometry[J]. https://doi.org/10.1016/j.foodchem.2018.07.068.
[31] STAHNKE H, KITTLAUS S, KEMPE G, ALDER L. Reduction of matrix effectsin liquid chromatography-electrospray ionization-mass spectrometry by dilution of the sample extracts:how much dilution is needed?[J]. Analytical Chemistry, 2012, 84(3): 1 474-1 482.
[32] FERRER C, LOZANO A, AGüERA A, GIRóN A J, FERNáNDEZ-ALBA A R. Overcoming matrix effects using the dilution approach in multiresiduemethods for fruits and vegetables[J]. Journal of Chromatography A, 2011, 1 218(42): 7 634-7 639.
[2] WU L M, CHEN L Z, SELVARAJ J N, WEI Y, WANG Y, LI Y, ZHAO J, XUE X F. Identification of the distribution of adenosine phosphates, nucleosides and nucleobases in royal jelly[J]. Food Chemistry, 2015, (173): 1 111-1 118.
[3] 中国医药保健品进出口商会. 2012年蜂王浆产品出口额创十年最高[J]. 中国蜂业,2013,(64):45-46. China Chamber of Commerce for Import & Export of Medicines & Health Products.In 2012,The highest level for export of royal jelly products in last ten years[J]. Apiculture of China, 2013, (64): 45-46(in Chinese).
[4] XU X, GAO Y X.Isolation and characterization of proteins and lipids from honeybee (Apismellifera L.) queen larvae and royal jelly[J]. Food Research International, 2013, 54(1): 330-337.
[5] PASTOR-BELDA M, GARRIDO I, CAMPILLO N, VI?AS P, HELLíN P, FLORES P, FENOLL J. Determination of spirocyclic tetronic/tetramic acid derivatives and neonicotinoid insecticides in fruits and vegetables by liquid chromatography and mass spectrometry after dispersive liquid-liquid microextraction[J]. Food Chemitry, 2016, (202): 389-395.
[6] CHAGNON M, KREUTZWEISER D, MITCHELL E A, MORRISSEY C A, NOOME D A, SLUIJS J P V. Risks of large scale use of systemic insecticides to ecosystem functioning and services[J]. Environmental Science and Pollution Research, 2012, 22(1): 119-134.
[7] LU C, WARCHOL K M, CALLAHAN R A. In situ replication of honey bee colony collapse disorder[J]. Bulletin of Insectology, 2012, 65(1): 99-106.
[8] LAURINO D, MANINO A, PATETTA A, PORPORATO M. Toxicity of neonicotinoid insecticides on different honey bee genotypes[J].Bulletin of Insectology, 2013, 66(1): 119-126.
[9] VICHAPONG J, BURAKHAM R, SRIJARANAI S. In-coupled syringe assisted octanol-water partition microextraction coupled with high-performance liquid chromatography for simultaneous determination of neonicotinoid insecticide residues in honey[J]. Talanta, 2015, (139): 21-26.
[10] MITCHELL E A D, MULHAUSER B, MULOT M, MUTABAZI A, GLAUSER G, AEBI A. A world wide survey of neonicotinoids in honey[J]. Science, 2017, 358(6 359): 109-111.
[11] The European Union. EU pesticides database[EB/OL]. https://ec.europa.eu/food/plant/pesticides/2018/05/01.
[12] Japan. Positive list system for agricultural chemical residues in foods[EB/OL]. http://www.mhlw.go.jp/english/topics/foodsafety/positivelist060228/2018/05/01.
[13] 许秀莹,施海燕,王鸣华. 气相色谱-质谱联用测定大米中种烟碱类农药残留[J]. 质谱学报,2012,33(2):99-103. XU Xiuying, SHI Haiyan, WANG Minghua.Determination of six neonicotinoid pesticides residue in rice by GC/MS[J]. Journal of Chinese Mass Spectrometry Society, 2012, 33(2): 99-103(in Chinese).
[14] GB/T 19648—2006 水果和蔬菜中500种农药及相关化学品残留量的测定气相色谱-质谱法[S]. 北京:中国标准出版社,2006.
[15] KO A Y, RAHMAN M M, ABD EL-ATY A M, JANG J, PARK J H, CHO S K, SHIM J H. Development of a simple extraction and oxidation procedure for the residue analysis of imidacloprid and its metabolites in lettuce using gas chromatography[J]. Food Chemistry, 2014, 148(3): 402-409.
[16] CAMPILLO N, VINAS P, FEREZ-MELGAREJO G, HERNANDEZ-CORDOBA M. Liquid chromatography with diode array detection and tandem mass spectrometry for the determination of neonicotinoid insecticides in honey samples using dispersive liquid-liquid microextraction[J]. Journal of Agricultural and Food Chemistry, 2013, (61): 4 799-4 805.
[17] 侯如燕,蔡荟梅,张正竹,宛晓春. 液相色谱法检测水果蔬菜中的烟碱类农药残留[J]. 分析试验室,2010,29(2):59-63. HOU Ruyan, CAI Huimei, ZHANG Zhengzhu, WAN Xiaochun.Determination of neonicotinoid pesticide residues in vegetables and fruits with high-performance liquid chromatography with diode-array detection[J]. Chinese Journal of Analysis Laboratory, 2010, 29(2): 59-63(in Chinese).
[18] 侯如燕,卞红正,赵秀霞,胡秭芳,苏婷,王孝辉,宛晓春. 固相萃取-液相色谱测定复杂基质蔬菜中 9种烟碱类残留[J]. 分析测试学报,2011,30(1):58-63. HOU Ruyan, BIAN Zhenghong, ZHAO Xiuxia, HU Zifang, SU Ting, WANG Xiaohui, WAN Xiaochun. Determination of nicotinoid residues in complicated matrix vegetables by solid phase extraction and HPLC method[J]. Journal of Instrumental Analysis, 2011, 30(1): 58-63(in Chinese).
[19] GARCíA M D, GALERA M M, VALVERDE R S, GALANTI A, GIROTTI S. Column switching liquid chromatography and post-column photochemically fluorescence detection to determine imidacloprid and 6-chloronicotinic acid in honeybees[J]. Journal of Chromatography A, 2007, (1 147): 17-23.
[20] RANCAN M, SABATINI A G, ACHILLI G, GALLETTI G C. Determination of imidacloprid and metabolites by liquid chromatography with an electrochemical detector and post column photochemical reactor[J]. Analytica Chimica Acta, 2006, 555(1): 20-24.
[21] 王东,侯传金,赵尔成,贾春虹. 盐析辅助均相液液萃取/分散固相萃取-超高效液相色谱串联质谱法测定蜂蜜中新烟碱类农药残留[J]. 分析测试学报,2015,34(6):681-685. WANG Dong, HOU Chuanjin, ZHAO Ercheng, JIA Chunhong.Determination of neonicotinoid residues in honey by ultra performance liquid chromatography-tandem mass spectrometry combined with salting-out homogeneous liquid-liquid extraction and dispersive solid-phase extraction[J]. Journal of Instrumental Analysis, 2015, 34(6): 681-685(in Chinese).
[22] 粟有志,李芳,齐鑫,史秀丽,王振宝. QuEChERS-高效液相色谱/串联质谱法同时测定蜂蜜中9种新烟碱类杀虫剂残留[J]. 分析科学学报,2015,31(2):203-207. SU Youzhi, LI Fang, QI Xin, SHI Xiuli, WANG Zhenbao. Determination of nine neonicotinoid insecticides in honey by QuEChERS-high performance liquid chromatography-tandem mass spectrometry[J]. Journal of Analytical Science, 2015, 31(2): 203-207(in Chinese).
[23] TANNER G, CZERWENKA C. LC-MS/MS Analysis of neonicotinoid insecticides in honey methodology and residue findings in Austrian honeys[J]. Journal of Agricultural and Food Chemistry, 2011, 59(23): 12 271-12 277.
[24] JIAO W T, XIAO Y, QIAN X S, TONG M M, HU Y Z, HOU R Y, HUA R M. Optimized combination of dilution and refined QuEChERS to overcome matrix effects of six types of tea for determination eight neonicotinoid insecticides by ultra performance liquid chromatograph-electrospray tandem mass spectrometry[J]. Food Chemistry, 2016, (210): 26-34.
[25] GBYLIK-SIKORSKA M, SNIEGOCKI T, POSYNIAK A. Determination of neonicotinoid insecticides and their metabolites in honey bee and honey by liquid chromatography tandem mass spectrometry[J]. Journal of Chromatography B, 2015, (990): 132-140.
[26] SUGANTHI A, BHUVANESWARI K, RAMYA M.Determination of neonicotinoid insecticide residues in sugarcane juice using LC-MS/MS[J]. Food Chemistry, 2018, (241): 275-280.
[27] GB/T 20769—2008 水果和蔬菜中450种农药及相关化学品残留量的测定液相色谱-串联质谱法[S]. 北京:中国标准出版社,2006.
[28] GB/T 23205—2008 茶叶中448种农药及相关化学品残留量的测定液相色谱-串联质谱法[S]. 北京:中国标准出版社,2008.
[29] VALVERDE S, ARES A M, ARRIBAS M, BERNAL J L, NOZAL M J. Development and validation of UHPLC-MS/MS methods for determination of neonicotinoid insecticides in royal jelly-based products[J]. Journal of Food Composition and Analysis, 2018, (70): 105-113.
[30] HOU J B, XIE W, HONG D, ZHANG W H, LI F, QIAN Y, HAN C. Simultaneous determination of ten neonicotinoid insecticides and two metabolites in honey and Royal-jelly by solid-phase extraction and liquid chromatography-tandem mass spectrometry[J]. https://doi.org/10.1016/j.foodchem.2018.07.068.
[31] STAHNKE H, KITTLAUS S, KEMPE G, ALDER L. Reduction of matrix effectsin liquid chromatography-electrospray ionization-mass spectrometry by dilution of the sample extracts:how much dilution is needed?[J]. Analytical Chemistry, 2012, 84(3): 1 474-1 482.
[32] FERRER C, LOZANO A, AGüERA A, GIRóN A J, FERNáNDEZ-ALBA A R. Overcoming matrix effects using the dilution approach in multiresiduemethods for fruits and vegetables[J]. Journal of Chromatography A, 2011, 1 218(42): 7 634-7 639.