超高效液相色谱-串联质谱测定酵素中14种常见杀菌剂残留
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摘要
目的建立分散固相萃取前处理技术结合超高效液相色谱-串联质谱法测定酵素中14种常见杀菌剂残留。方法酵素样品经乙腈提取、分散固相萃取吸附剂除去色素、多糖等干扰物。采用C_(18)色谱柱分离后,用超高效液相色谱-串联质谱于电喷雾正离子源和多反应监测扫描模式下进行测定,基质匹配标准曲线外标法定量。结果 14种目标化合物在20、50、100mg/kg加标水平下,回收率为81.0%～100.3%,相对标准偏差在5.7%～12.3%之间。14种目标化合物的检出限在0.2～0.7mg/kg之间,定量限在0.5～2.0mg/kg之间。结论该方法前处理简单、快速,灵敏度和准确度高,包含种类较宽,具有一定的拓展性,适用于酵素中杀菌剂残留的日常监测。
Objective To establish an analytical method for determination of 14 kinds of common fungicide residues in leaven by dispersive solid phase extraction-ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). Methods Leaven samples were extracted with acetonitrile, purified by dispersive solid phase extraction to remove interfering substances such as colorings and polysaccharide. The separation was performed on a C_(18) column, then the 14 kinds of fungicides were detected by ultra performance liquid chromatography-tandem mass spectrometry with ESI positive ion scan in mode of multiple reaction monitoring(MRM) and quantified by matrix-matched external standard method. Results At the spiked level of 20, 50 and 100μg/kg, the recoveries of each compound were in the range of 81.0%-100.3% with the relative standard deviations of5.7%-12.3%. The limits of detections were 0.3-0.7 μg/kg and the limits of quantitative were 0.5-2.0 μg/kg for the 14 targets compounds. Conclusion This method is simple, rapid, high sensitivity and good stability, with a wide variety and a certain development. It can be used for the daily monitoring of fungicides in leaven.
Objective To establish an analytical method for determination of 14 kinds of common fungicide residues in leaven by dispersive solid phase extraction-ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). Methods Leaven samples were extracted with acetonitrile, purified by dispersive solid phase extraction to remove interfering substances such as colorings and polysaccharide. The separation was performed on a C_(18) column, then the 14 kinds of fungicides were detected by ultra performance liquid chromatography-tandem mass spectrometry with ESI positive ion scan in mode of multiple reaction monitoring(MRM) and quantified by matrix-matched external standard method. Results At the spiked level of 20, 50 and 100μg/kg, the recoveries of each compound were in the range of 81.0%-100.3% with the relative standard deviations of5.7%-12.3%. The limits of detections were 0.3-0.7 μg/kg and the limits of quantitative were 0.5-2.0 μg/kg for the 14 targets compounds. Conclusion This method is simple, rapid, high sensitivity and good stability, with a wide variety and a certain development. It can be used for the daily monitoring of fungicides in leaven.
引文
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[17]侯雪,韩梅,邱世婷,等.改进的QuEChERS气相色谱-串联质谱法测定草莓中21种杀菌剂残留[J].农药学学报,2017,19(1):46-52.Hou X,Han M,Qiu ST,et al.Residues of 21 fungicides in Fragaria ananassa by modified QuEChERS and gas chromatography-tandem mass spectrometry[J].Chin J Pest Sci,2017,19(1):46-52.
[18]许欣欣,王冰,陈慧玲,等.超高效液相色谱-串联质谱法同时测定水果蔬菜中11种杀菌剂[J].食品安全质量检测学报,2018,9(1):141-148.Xu XX,Wang B,Chen HL,et al.Simultaneous determination of 11 kinds of fungicides in fruit and vegetable by ultra performance liquid chromatography-tandem mass spectrometry[J]J Food Saf Qual,2018,9(1):141-148.
[19]师真,陈俊秀,李旭.高效液相色谱-串联质谱法测定蔬菜中13种氨基甲酸酯类农药和杀菌剂残留[J].食品安全质量检测学报,2018,9(20):5439-5445.Shi Z,Chen JX,Li X.Determination of 13 kinds of carbamate pesticides and fungicides in vegetables by high performance liquid chromatographytandem mass spectrometry[J].J Food Saf Qual,2018,9(20):5439-5445.
[2]唐超,江惠娟,苏二正.食用酵素的研究进展[J].生物加工过程,2018,16(3):84-90.Tang C,Jiang HJ,Su EZ.Research progress of edible Jiaosu[J].Chin JBioprocess Eng,2018,16(3):84-90.
[3]沈燕飞,聂小华,孟祥河,等.酵素食品加工微生物与功能特性研究进展[J].浙江农业科学,2019,60(1):112-116.Shen YF,Nie XH,Meng XH,et al.Research progress on microorganism and functional characteristics of enzyme food processing[J].J Zhejiang Agric Sci,2019,60(1):112-116.
[4]Feng Y,Zhang M,Mujumdr AS,et al.Recent research process of fermented plant extract:A review[J].Trends Food Sci Technol,2017,65:40-48.
[5]Hornero-Méndez D,Cerrillo I,Ortega,et al.?-Cryptoxanthin is more bioavailable in human from fermented orange juice than from orange juice[J].Food Chem,2018,262:215-220.
[6]Lin YL,Lin HW,Chen YC,et al.Hepatoprotective effects of naturally fermented noni juice against thioacetamide-induced liver fibrosis in rats[J].J Chin Med,2017,80(4):212-221.
[7]Li C,Nie SP,Zhu KX,et al.Lactobacillus plantarum NCU116 fermented carrot juice evokes changes of metabolites in serum from type 2 diabetic rats[J].Food Res Int,2016,80:36-40.
[8]Garcia-diaz DF,Johnson MH,De-Mejia EG.Anthocyanins from fermented berry beverages inhibit inflammation-related adiposity response in vitro[J].J Med Food,2015,18(4):489-496.
[9]Kwaw E,Ma Y,Tchabo W,et al.Effects of lactobacillus strains on phenolic profile,color attributes and antioxidant activities of lactic-acid-fermented mulberry juice[J].Food Chem,2018,1:148-154.
[10]陈海明,李慧,王璐芳,等.分散固相萃取-气相色谱-串联质谱法同时测定草莓及土壤中5种杀菌剂[J].食品安全质量检测学报,2018,9(24):7471-6477.Chen HM,Li H,Wang LF,et al.Simultaneous determination of five fungicides in strawberry and soil by dispersive solid phase extraction-gas chromatography-tandem mass spectrometry[J].J Food Saf Qual,2018,9(24):7471-6477.
[11]Schenck FJ,Lehotay SJ,Vega V.Comparison of solid-phase extraction sorbents for cleanup in pesticide residue analysis of fresh fruits and vegetables[J].J Sep Sci,2015,25(14):883-890.
[12]赵春娟,庞军,高文惠.分子印迹固相萃取-高效液相色谱法分析食品中3种三唑类杀菌剂残留[J].中国食品学报,2015,15(3):175-180.Zhao CJ,Pang J,Gao WH.Analysis of Three Triazole Fungicide Residues in Food by Molecularly Imprinted Solid Phas Extraction-HPLC[J].J Chin Inst Food Sci Technol,2015,15(3):175-180.
[13]王璐芳,李春梅,许佳彬,等.QuEChERS超高效液相色谱串联质谱法测定不同植被类型土壤中11种甲氧基丙烯酸酯类杀菌剂[J].色谱,2018,36(8):730-737.Wang LF,Li CM,Xu JB,et al.Simultaneous determination of 11strobilurin fungicides in different vegetation types of soil by Qu ECh ERS-ultra performance liquid chromatography-tandem mass spectrometry[J].Chin J Chromatogr,2018,36(8):730-737.
[14]吴南村,张群,刘春华,等.QuEChERS-气相色谱串联质谱法检测诺丽酵素原液中12种农药残留[J].湖北农业科学,2019,58(1):96-99.Wu NC,Zhang Q,Liu CH,et al.Simultaneous determination of fermentation broth of morinda citrifolia using QuEChERS-Gas chromatography-tandem mass spectrometry[J].Hubei Agric Sci,2019,58(1):96-99.
[15]Golge O,Koluman A,Kabak B.Validation of a modified QuEChERSmethod for the determination of 167 pesticides in milk and milk products by LC-MS/MS[J].Food Anal Method,2017,11(1):1-27.
[16]Liu XQ,Li YF,Meng WT,et al.A multi-residue method for simultaneous determination of 74 pesticides in Chinese material medica using modified QuEChERS sample preparation procedure and gas chromatography tandem mass spectrometry[J].J Chromatogr B,2016,1015:1-12.
[17]侯雪,韩梅,邱世婷,等.改进的QuEChERS气相色谱-串联质谱法测定草莓中21种杀菌剂残留[J].农药学学报,2017,19(1):46-52.Hou X,Han M,Qiu ST,et al.Residues of 21 fungicides in Fragaria ananassa by modified QuEChERS and gas chromatography-tandem mass spectrometry[J].Chin J Pest Sci,2017,19(1):46-52.
[18]许欣欣,王冰,陈慧玲,等.超高效液相色谱-串联质谱法同时测定水果蔬菜中11种杀菌剂[J].食品安全质量检测学报,2018,9(1):141-148.Xu XX,Wang B,Chen HL,et al.Simultaneous determination of 11 kinds of fungicides in fruit and vegetable by ultra performance liquid chromatography-tandem mass spectrometry[J]J Food Saf Qual,2018,9(1):141-148.
[19]师真,陈俊秀,李旭.高效液相色谱-串联质谱法测定蔬菜中13种氨基甲酸酯类农药和杀菌剂残留[J].食品安全质量检测学报,2018,9(20):5439-5445.Shi Z,Chen JX,Li X.Determination of 13 kinds of carbamate pesticides and fungicides in vegetables by high performance liquid chromatographytandem mass spectrometry[J].J Food Saf Qual,2018,9(20):5439-5445.