凝胶渗透色谱净化-液相色谱-同位素稀释串联质谱法测定肉及肉制品中的甲萘威残留
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摘要
称取试样约5g(精确至0.01g),加入1.000 mg·L~(-1)甲萘威-D7同位素内标溶液50μL,加入适量水(肉样加水1.5mL,肉制品加水3mL),加40mL丙酮,均质1min,加氯化钠6g,充分摇匀,再加30mL石油醚,振摇30min,静置30min。取有机层上清液,经无水硫酸钠过滤,旋转蒸发浓缩至约1mL,加2mL乙酸乙酯-环己烷(1+1)混合液,再浓缩至约1mL,如此重复3次。用乙酸乙酯-环己烷(1+1)溶液定容至10.0mL,经0.22μm滤膜过滤,进行凝胶色谱(GPC)净化。GPC条件如下:Bio Beads S-X3凝胶色谱净化柱(400mm×30mm),乙酸乙酯-环己烷(1+1)混合液为流动相,馏分收集段10.0～15.0min,在线浓缩加热温度45℃,真空度2.0×10~4Pa。以乙腈为替换溶剂替换两次后将净化液定容至1.0mL,进行液相色谱-串联质谱分析。采用HSS T3色谱柱(100mm×2.1mm,1.7μm)进行分离,以0.1%(体积分数)甲酸溶液-乙腈(6+4)为流动相,质谱分析中采用电喷雾正离子源和多反应监测模式。甲萘威的质量浓度在0.010～0.500mg·L~(-1)内和其峰面积与内标峰面积之比呈线性关系,测定下限(10S/N)为0.005mg·kg~(-1)。加标回收率在81.0%～105%之间,测定值的相对标准偏差(n=6)在3.8%～16%之间。
About 5 g(accurate to 0.01 g) of the sample and 50μL of 1.000 mg·L~(-1) carbaryl-D7 isotope internal standard solution were added into appropriate amount of water(1.5 mL of water for the meat sample,3 mL of water for meat products).Then 40 mL of acetone was added and the mixture was homogenized for 1 min.6 g of sodium chloride was added and the mixture was shaked well.30 mL of petroleum ether was added and the mixture was shaked for 30 min and let stand for 30 min.The organic layer supernatant was taken,filtered through anhydrous sodium sulfate,and concentrated to about 1 mL by rotary evaporation.2 mL of ethyl acetate-cyclohexane(1+1) solution was added,and the mixture was concentrated to about 1 mL by rotary evaporation.After the above operation was repeated 3 times,the solution was made to 10.0 mL with ethyl acetate-cyclohexane(1+1) solution,filtered through a 0.22μm filter membrane,and cleaned up by gel permeation chromatography(GPC) under conditions as follow:Bio Beads S-X3 gel chromatographic column(400 mm×30 mm) was used as stationary phase,with ethyl acetate-cyclohexane(1+1)solution as mobile phase;fraction collection section was 10.0-15.0 min;online concentration heating temperature was 45℃;degree of vacuum was 2.0×10~4 Pa.After solvent replacement was carried out 2 times with acetonitrile as replacement solvent,the purified solution was made up to to 1.0 mL,and analyzed by liquid chromatography-tandem mass spectrometry.Separation was performed on a HSS T3 column(100 mm×2.1 mm,1.7μm) with a mixture of 0.1%(volume fraction) formic acid solution-acetonitrile(6+4) as mobile phase.Electrospray ionization source and multiple reaction mornitoring mode were used in mass spectrometry.Linear relationship was found between the ratio of peak area of carbaryl to peak area of internal standard with the mass concentration of carbaryl in the range of 0.010-0.500 mg·L~(-1).The lower limit of determination(10 S/N) was 0.005 mg·kg~(-1).Values of recovery obtained by standard addition method were in the range of 81.0%-105%,the relative standard deviations(n=6) of the measured values were between 3.8% and16%.
About 5 g(accurate to 0.01 g) of the sample and 50μL of 1.000 mg·L~(-1) carbaryl-D7 isotope internal standard solution were added into appropriate amount of water(1.5 mL of water for the meat sample,3 mL of water for meat products).Then 40 mL of acetone was added and the mixture was homogenized for 1 min.6 g of sodium chloride was added and the mixture was shaked well.30 mL of petroleum ether was added and the mixture was shaked for 30 min and let stand for 30 min.The organic layer supernatant was taken,filtered through anhydrous sodium sulfate,and concentrated to about 1 mL by rotary evaporation.2 mL of ethyl acetate-cyclohexane(1+1) solution was added,and the mixture was concentrated to about 1 mL by rotary evaporation.After the above operation was repeated 3 times,the solution was made to 10.0 mL with ethyl acetate-cyclohexane(1+1) solution,filtered through a 0.22μm filter membrane,and cleaned up by gel permeation chromatography(GPC) under conditions as follow:Bio Beads S-X3 gel chromatographic column(400 mm×30 mm) was used as stationary phase,with ethyl acetate-cyclohexane(1+1)solution as mobile phase;fraction collection section was 10.0-15.0 min;online concentration heating temperature was 45℃;degree of vacuum was 2.0×10~4 Pa.After solvent replacement was carried out 2 times with acetonitrile as replacement solvent,the purified solution was made up to to 1.0 mL,and analyzed by liquid chromatography-tandem mass spectrometry.Separation was performed on a HSS T3 column(100 mm×2.1 mm,1.7μm) with a mixture of 0.1%(volume fraction) formic acid solution-acetonitrile(6+4) as mobile phase.Electrospray ionization source and multiple reaction mornitoring mode were used in mass spectrometry.Linear relationship was found between the ratio of peak area of carbaryl to peak area of internal standard with the mass concentration of carbaryl in the range of 0.010-0.500 mg·L~(-1).The lower limit of determination(10 S/N) was 0.005 mg·kg~(-1).Values of recovery obtained by standard addition method were in the range of 81.0%-105%,the relative standard deviations(n=6) of the measured values were between 3.8% and16%.
引文
[1] 达晶,王钢力,曹进,等.QuEChERS-液相色谱-串联质谱法测定植物性食品中30种氨基甲酸酯类农药残留[J].色谱,2015,33(8):830-837.
[2] 余宇成,方灵,苏德森,等.气相色谱-串联质谱法测定乌龙茶中5种氨基甲酸酯类农药[J]分析测试学报,2016,35(12):1586-1590.
[3] 吴刚,王华雄,俞春燕,等.加速溶剂萃取-GPC液相色谱柱后衍生化测定动物源性食品中多种氨基甲酸酯类农药残留量[J].中国食品卫生杂志,2008,20(5):409-413.
[4] (EU) No 1096/2014 Amending Annexes II,III and V to Regulation(EC) No 396/2005of the European Parliament and of the Council as regards maximum residue levels for carbaryl,procymidone and profenofos in or on certain products[S].
[5] 王丽敏,张静恒,喻秀,等.气相色谱-串联质谱测定蔬菜水果中克百威、3-羟基克百威和甲萘威残留[J].农药,2014,53(4):269-271.
[6] 卢丽明,丘福保,黄诚,等.高效液相色谱-柱后衍生法测定生活饮用水中呋喃丹、甲萘威[J].环境卫生学杂志,2014,4(4):403-406.
[7] 樊雯娟,代立勤,刘新智.高效液相色谱-柱后衍生法检测牛奶中10种氨基甲酸酯类农药残留[J].农产品加工,2016,1:29-34.
[8] 甘凤娟,陈砚朦,李月欢,等.高效液相色谱-柱后衍生荧光法检测氨基甲酸酯类农药残留量[J].中国卫生检验杂志,2005,15(12):1460-1461.
[9] 罗小玲,刘长勇.高效液相色谱法测定果蔬饮料中的克百威和甲萘威农药残留[J].食品科学,2009,30(8):245-246.
[10] 胡红芳,刘全斌,苏璞,等.快速溶剂萃取-液相色谱法测定大豆中甲萘威残留[J].解放军预防医学杂志,2014,32(5):459-459.
[11] 徐娟,陈捷,叶弘毅,等.QuEChERS提取与高效液相色谱-电喷雾电离串联质谱联用法检测茶叶中的19种农药残留[J].分析测试学报,2011,30(9):990-995.
[12] 徐文娟,王振刚,丁葵英,等.QuEChERS/液相色谱-串联质谱法测定5种蔬菜中17种氨基甲酸酯类农药的基质效应研究[J].分析测试学报,2017,36(1):54-60.
[13] 吕东晋,李瑛,曹海兰.凝胶渗透色谱净化液相色谱-串联质谱法检测袋泡茶中的8种氨基甲酸酯类农药残留[J].现代预防医学,2014,41(7):1280-1283.
[14] 王敬,陈瑞春,郭春海,等.液相色谱-串联质谱法测定植物源性食品中16种氨基甲酸酯类农药及其代谢物[J].食品安全质量检测学报,2013,4(5):92-98.
[15] 支建梁.同位素稀释质谱在食品与环境分析中的应用[J].粮食与食品工业,2010,17(5):61-64.
[16] GB 5009.163-2003 动物性食品中氨基甲酸酯类农药多组分残留高效液相色谱测定[S].
[17] GB 23200.105-2016 肉及肉制品中甲萘威残留量的测定液相色谱-柱后衍生荧光检测法[S].
[2] 余宇成,方灵,苏德森,等.气相色谱-串联质谱法测定乌龙茶中5种氨基甲酸酯类农药[J]分析测试学报,2016,35(12):1586-1590.
[3] 吴刚,王华雄,俞春燕,等.加速溶剂萃取-GPC液相色谱柱后衍生化测定动物源性食品中多种氨基甲酸酯类农药残留量[J].中国食品卫生杂志,2008,20(5):409-413.
[4] (EU) No 1096/2014 Amending Annexes II,III and V to Regulation(EC) No 396/2005of the European Parliament and of the Council as regards maximum residue levels for carbaryl,procymidone and profenofos in or on certain products[S].
[5] 王丽敏,张静恒,喻秀,等.气相色谱-串联质谱测定蔬菜水果中克百威、3-羟基克百威和甲萘威残留[J].农药,2014,53(4):269-271.
[6] 卢丽明,丘福保,黄诚,等.高效液相色谱-柱后衍生法测定生活饮用水中呋喃丹、甲萘威[J].环境卫生学杂志,2014,4(4):403-406.
[7] 樊雯娟,代立勤,刘新智.高效液相色谱-柱后衍生法检测牛奶中10种氨基甲酸酯类农药残留[J].农产品加工,2016,1:29-34.
[8] 甘凤娟,陈砚朦,李月欢,等.高效液相色谱-柱后衍生荧光法检测氨基甲酸酯类农药残留量[J].中国卫生检验杂志,2005,15(12):1460-1461.
[9] 罗小玲,刘长勇.高效液相色谱法测定果蔬饮料中的克百威和甲萘威农药残留[J].食品科学,2009,30(8):245-246.
[10] 胡红芳,刘全斌,苏璞,等.快速溶剂萃取-液相色谱法测定大豆中甲萘威残留[J].解放军预防医学杂志,2014,32(5):459-459.
[11] 徐娟,陈捷,叶弘毅,等.QuEChERS提取与高效液相色谱-电喷雾电离串联质谱联用法检测茶叶中的19种农药残留[J].分析测试学报,2011,30(9):990-995.
[12] 徐文娟,王振刚,丁葵英,等.QuEChERS/液相色谱-串联质谱法测定5种蔬菜中17种氨基甲酸酯类农药的基质效应研究[J].分析测试学报,2017,36(1):54-60.
[13] 吕东晋,李瑛,曹海兰.凝胶渗透色谱净化液相色谱-串联质谱法检测袋泡茶中的8种氨基甲酸酯类农药残留[J].现代预防医学,2014,41(7):1280-1283.
[14] 王敬,陈瑞春,郭春海,等.液相色谱-串联质谱法测定植物源性食品中16种氨基甲酸酯类农药及其代谢物[J].食品安全质量检测学报,2013,4(5):92-98.
[15] 支建梁.同位素稀释质谱在食品与环境分析中的应用[J].粮食与食品工业,2010,17(5):61-64.
[16] GB 5009.163-2003 动物性食品中氨基甲酸酯类农药多组分残留高效液相色谱测定[S].
[17] GB 23200.105-2016 肉及肉制品中甲萘威残留量的测定液相色谱-柱后衍生荧光检测法[S].