基于QuEChERS-四级杆/静电场轨道阱高分辨质谱法测定酱油类调味品中的氨基甲酸乙酯
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摘要
建立四级杆/静电场轨道阱高分辨质谱检测酱油类调味品中氨基甲酸乙酯的方法。样品采用乙腈提取,经优化后的QuEChERS方法净化后,用高分辨质谱QExactive进行测定。该实验对目标物二级特征碎片进行同位素匹配,推测断裂规律,并对不同酱油类样品完成基质效应评价。结果表明:该方法在1～20μg/L范围内的线性范围良好,精密度与准确度高,检出限达到1.5μg/kg,4种不同类酱油对均无基质效应,适用于酱油中氨基甲酸乙酯的快速检测与确证分析。
A new method for direct determination of ethyl carbamate in soy sauce by quadrupole electrostatic field orbitrap high-resolution mass spectrometry is established. The sample is extracted with acetonitrile, purified by optimized QuEChERS method and determined by HRMS QExactive. The secondary feature fragments of the target compound are utilized with isotope distribution. The fracture rule is predicted and the matrix effect of different soy sauce samples is evaluated. The results show that this method has good linearity in the range of 1～20 μg/L. The method has high precision and accuracy, the limit of detection is 1.5 μg/kg, satisfying the detection demands. This method is suitable for the rapid determination and confirmatory analysis of ethyl carbamate in soy sauce.
A new method for direct determination of ethyl carbamate in soy sauce by quadrupole electrostatic field orbitrap high-resolution mass spectrometry is established. The sample is extracted with acetonitrile, purified by optimized QuEChERS method and determined by HRMS QExactive. The secondary feature fragments of the target compound are utilized with isotope distribution. The fracture rule is predicted and the matrix effect of different soy sauce samples is evaluated. The results show that this method has good linearity in the range of 1～20 μg/L. The method has high precision and accuracy, the limit of detection is 1.5 μg/kg, satisfying the detection demands. This method is suitable for the rapid determination and confirmatory analysis of ethyl carbamate in soy sauce.
引文
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[6]周雪燕,辛敏汉,肖婧,等.产氨基甲酸乙酯降解酶酵母菌的筛选鉴定及发酵条件优化[J].中国调味品,2019,44(3):5-10.
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[9]Viera M S,Rizzetti T M,De-souza M P,et al.Multiresidue determination of pesticides in crop plants by the quick,easy,cheap,effective,rugged,and safe method and ultra-high-performance liquid chromatography tandem mass spectrometry using a calibration based on a single level standard addition in the sample[J].J Chromatogr A,2017,1526:119-127.
[10]Liu M,Xie Y,Li H Y,et al.Multiresidue determination of 29 pesticide residues in pepper through a modified QuEChERS method and gas chromatography-mass spectrometry[J].Biomedical Chromatography,2016,30(10):1686-1695.
[11]Besil N,Cesio V,Heinzen H,et al.Matrix effects and interferences of different citrus fruit co-extractives in pesticide residue analysis using ultrahigh-performance liquid chromatography-high-resolution mass spectrometry[J].Journal of Agricultural and Food Chemistry,2017,65:4819-4829.
[12]Ferrer C,Lozano A,Aguera A,et al.Overcoming matrix effects using the dilution approach in multiresidue methods for fruits and vegetables[J].J Chromatogr,2011,12(18):7634-7639.
[13]王成龙,黄秋婷,戚平.超高效液相色谱-四级杆/静电场轨道阱高分辨质谱法对酒中氨基甲酸乙酯确认分析的研究[J].酿酒科技,2016(7):112-115.
[14]王成龙,赵金利,李燕莹,等.超高效液相色谱-四级杆静电场轨道肼高分辨质谱测定聚丙烯酰胺中丙烯酰胺单体的残留[J].色谱,2017(12):1294-1300.
[2]信海红,王媛媛,洪思慧,等.基于风险矩阵的酱油质量安全风险评价[J].中国调味品,2015,40(5):46-49,56.
[3]姚晓瑞宁,高飞飞,王斌,等.产氨基甲酸乙酯降解酶酵母菌的选育及产酶条件优化[J].中国调味品,2018,43(1):43-47.
[4]谢承佳.酱油中的有害成分及其检测技术研究进展[J].中国调味品,2015,40(6):132-136.
[5]李晓芹,金尉,袁小美,等.GC-MS内标法测定发酵食品中氨基甲酸乙酯的含量[J].中国调味品,2017,42(6):135-138.
[6]周雪燕,辛敏汉,肖婧,等.产氨基甲酸乙酯降解酶酵母菌的筛选鉴定及发酵条件优化[J].中国调味品,2019,44(3):5-10.
[7]Anastassiades M,Lehotay S J,Stajnbaher D,et al.Fast and easy multi-residue method employing acetonitrile extraction/partitioning an "dispersive solid-phase extraction" for the determination of pesticide residues in produce[J].Journal of AOAC International,2003,86(2):412-431.
[8]Manav ? G,Dinc-Zor S,Alpdogan G.Optimization of a modified QuEChERS method by means of experimental design for multiresidue determination of pesticides in milk and dairy products by GC-MS[J].Microchem J,2019,144:124-129.
[9]Viera M S,Rizzetti T M,De-souza M P,et al.Multiresidue determination of pesticides in crop plants by the quick,easy,cheap,effective,rugged,and safe method and ultra-high-performance liquid chromatography tandem mass spectrometry using a calibration based on a single level standard addition in the sample[J].J Chromatogr A,2017,1526:119-127.
[10]Liu M,Xie Y,Li H Y,et al.Multiresidue determination of 29 pesticide residues in pepper through a modified QuEChERS method and gas chromatography-mass spectrometry[J].Biomedical Chromatography,2016,30(10):1686-1695.
[11]Besil N,Cesio V,Heinzen H,et al.Matrix effects and interferences of different citrus fruit co-extractives in pesticide residue analysis using ultrahigh-performance liquid chromatography-high-resolution mass spectrometry[J].Journal of Agricultural and Food Chemistry,2017,65:4819-4829.
[12]Ferrer C,Lozano A,Aguera A,et al.Overcoming matrix effects using the dilution approach in multiresidue methods for fruits and vegetables[J].J Chromatogr,2011,12(18):7634-7639.
[13]王成龙,黄秋婷,戚平.超高效液相色谱-四级杆/静电场轨道阱高分辨质谱法对酒中氨基甲酸乙酯确认分析的研究[J].酿酒科技,2016(7):112-115.
[14]王成龙,赵金利,李燕莹,等.超高效液相色谱-四级杆静电场轨道肼高分辨质谱测定聚丙烯酰胺中丙烯酰胺单体的残留[J].色谱,2017(12):1294-1300.