超高效液相色谱-串联质谱法同时测定水果中8种杀菌剂残留
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摘要
目的建立水果中甲基硫菌灵、甲霜灵、烯酰吗啉、嘧霉胺、三唑酮、苯醚甲环唑、咪鲜胺、多菌灵8种杀菌剂的超高效液相色谱-串联四级杆质谱(UHPLC-MS/MS)检测方法。方法样品采用含有1%乙酸的乙腈溶液提取,无水硫酸镁-醋酸钠盐析,提取液1∶9稀释后,采用Agilent ZORBAX XDB C18色谱柱(100 mm×2. 1 mm,1. 8μm),梯度洗脱,采用MRM模式测定,外标法定量。结果 8种目标物质在给定的浓度范围内具有良好的线性关系(r≥0. 999 0),方法定量限为0. 000 6 mg/kg～0. 006 mg/kg,加标回收率为84. 6%～104. 2%,相对标准偏差(RSD)均<5. 4%。结论本方法改良了QuRCh ERS的样品前处理技术,操作简单,定量准确可靠,具有良好的灵敏度、回收率和重复性,适合水果中杀菌剂的测定。
Objective An ultra-performance liquid chromatography-tandem mass spectrometry( UHPLC-MS/MS) method was developed to determine 8 fungicide residues such as methyl-thiazolam,metazolam,enommorpholine,pyrimethanil,triazolone,phenylethoxazole,imisumide,carbendazim. Methods The fruits samples were extracted by acetonitrile containing1% acetic acid,and salted out with anhydrous magnesium-sodium chloride. After the crude extract was diluted 10 times,the target analytes were separated on a Agilent ZORBAX XDB C18 column( 100 mm × 2. 1 mm,1. 8 μm) with gradient elution using acetonitrile and water. The samples were detected by tandem quadrupole mass spectrometry with multiple reaction monitoring( MRM). External standard method was used to calibrate the results. Results Good linearities were achieved for all analytes with correlation coefficient( r) above 0. 999 0. The quantitation limits of the method( LOQ) were within0. 000 6 mg/kg-0. 006 mg/kg. The recoveries of the target analytes ranged from 84. 6% to 104. 2%,with relative standard deviations( RSD) less than 5. 4%. Conclusion This method improved the sample pretreatment technology of QuRCh ERS. It is simple,accurate and reliable for determination of 8 fungicide residues in fruits
Objective An ultra-performance liquid chromatography-tandem mass spectrometry( UHPLC-MS/MS) method was developed to determine 8 fungicide residues such as methyl-thiazolam,metazolam,enommorpholine,pyrimethanil,triazolone,phenylethoxazole,imisumide,carbendazim. Methods The fruits samples were extracted by acetonitrile containing1% acetic acid,and salted out with anhydrous magnesium-sodium chloride. After the crude extract was diluted 10 times,the target analytes were separated on a Agilent ZORBAX XDB C18 column( 100 mm × 2. 1 mm,1. 8 μm) with gradient elution using acetonitrile and water. The samples were detected by tandem quadrupole mass spectrometry with multiple reaction monitoring( MRM). External standard method was used to calibrate the results. Results Good linearities were achieved for all analytes with correlation coefficient( r) above 0. 999 0. The quantitation limits of the method( LOQ) were within0. 000 6 mg/kg-0. 006 mg/kg. The recoveries of the target analytes ranged from 84. 6% to 104. 2%,with relative standard deviations( RSD) less than 5. 4%. Conclusion This method improved the sample pretreatment technology of QuRCh ERS. It is simple,accurate and reliable for determination of 8 fungicide residues in fruits
引文
[1]王菲,李彤,马辰.超高效液相色谱-串联质谱法测定中药材中的三唑类杀菌剂及三嗪类除草剂的残留量[J].色谱,2013,31(3):191-199.
[2]沈伟健,桂茜雯,余可倥,等.气相色谱-负化学离子源质谱测定大豆和玉米中12种三唑类杀菌剂的残留量[J].色谱,2009,27(1):91-95.
[3]林维宣.各国食品中农药兽药残留量规定[M].大连:大连海事大学出版社,2012:1018-1025.
[4]中华人民共和国国家卫生和计划生育委员会,中华人民共和国农业部. GB 2763—2014食品安全国家标准食品中农药最大残留限量[S].北京:中国标准出版社,2014.
[5]史龙梅,李欢,周建科.液相色谱法检测番茄汁中杀菌剂和杀虫剂的研究[J].食品与发酵科技,2014,50(6):70-73.
[6]杨欢,孙伟华,曹赵云,等.改良QuRChERS方法快速测定国蔬中8种新型琥珀酸脱氢酶抑制剂类杀菌剂[J].色谱,2016,34(11):1070-1076.
[7]东保柱,王振,景岚,等. HPLC法同时检测土壤中多菌灵、菌核净、速克灵、咪鲜胺4种杀菌剂[J].农药,2016,55(3):205-207.
[8]乐渊,张群,刘春华,等. QuRChERS净化超高效液相色谱-串联质谱法检测莲雾中4种杀菌剂[J].分析科学学报,2016,32(3):409-413.
[9]王云风,葛宝坤,高建会,等.液相色谱-质谱法测定果蔬中8种甲氧丙烯酸酯类杀菌剂残留量[J].食品研究与开发,2009,30(4):130-133.
[10]孙亚米,吕燕,吴银良,等.液相色谱-串联质谱法快速测定果蔬中16种新型酰胺类杀菌剂残留量[J].食品科学,2015,36(12):230-237.
[11]陈小龙,李正翔,曹赵云,等.液相色谱-串联质谱法测定蔬菜和水果中6种新型酰胺类杀菌剂残留量[J].色谱,2013,31(10):954-960.
[12]齐沛沛,范旭,周莉,等.基于超高效液相色谱-串联质谱快速测定草莓中典型杀菌剂[J].浙江农业科学,2015,56(6):871-874.
[13]王玉健,庞道标,黄惠玲,等.高效液相色谱-串联质谱法同时测定蔬菜中4种杀菌剂的残留量[J].食品工业,2015,36(5):290-295.
[14]魏畅,傅红,郑俊超,等. QuRChERS-液质联用同步检测蘑菇中多菌灵等3种杀菌剂残留[J].食品工业,2016,16(11):189-195.
[15]张榕杰,张伟,马青青.超高效液相色谱-串联质谱法同时测定水果中9种杀菌剂的残留量[J].中国卫生检验杂志,2015,25(18):3080-3083.
[16]沈伟健,毛应民,吴斌.气相色谱-正化学源-质谱联用技术测定葡萄和葡萄酒中多种唑类杀菌剂的残留量[J].分析化学,2010,38(7):941-947.
[17] Matuszewski BK,Constanzer ML,Chavez-Eng CM. Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS[J]. Anal Chem,2003,75(13):3019-3030.
[2]沈伟健,桂茜雯,余可倥,等.气相色谱-负化学离子源质谱测定大豆和玉米中12种三唑类杀菌剂的残留量[J].色谱,2009,27(1):91-95.
[3]林维宣.各国食品中农药兽药残留量规定[M].大连:大连海事大学出版社,2012:1018-1025.
[4]中华人民共和国国家卫生和计划生育委员会,中华人民共和国农业部. GB 2763—2014食品安全国家标准食品中农药最大残留限量[S].北京:中国标准出版社,2014.
[5]史龙梅,李欢,周建科.液相色谱法检测番茄汁中杀菌剂和杀虫剂的研究[J].食品与发酵科技,2014,50(6):70-73.
[6]杨欢,孙伟华,曹赵云,等.改良QuRChERS方法快速测定国蔬中8种新型琥珀酸脱氢酶抑制剂类杀菌剂[J].色谱,2016,34(11):1070-1076.
[7]东保柱,王振,景岚,等. HPLC法同时检测土壤中多菌灵、菌核净、速克灵、咪鲜胺4种杀菌剂[J].农药,2016,55(3):205-207.
[8]乐渊,张群,刘春华,等. QuRChERS净化超高效液相色谱-串联质谱法检测莲雾中4种杀菌剂[J].分析科学学报,2016,32(3):409-413.
[9]王云风,葛宝坤,高建会,等.液相色谱-质谱法测定果蔬中8种甲氧丙烯酸酯类杀菌剂残留量[J].食品研究与开发,2009,30(4):130-133.
[10]孙亚米,吕燕,吴银良,等.液相色谱-串联质谱法快速测定果蔬中16种新型酰胺类杀菌剂残留量[J].食品科学,2015,36(12):230-237.
[11]陈小龙,李正翔,曹赵云,等.液相色谱-串联质谱法测定蔬菜和水果中6种新型酰胺类杀菌剂残留量[J].色谱,2013,31(10):954-960.
[12]齐沛沛,范旭,周莉,等.基于超高效液相色谱-串联质谱快速测定草莓中典型杀菌剂[J].浙江农业科学,2015,56(6):871-874.
[13]王玉健,庞道标,黄惠玲,等.高效液相色谱-串联质谱法同时测定蔬菜中4种杀菌剂的残留量[J].食品工业,2015,36(5):290-295.
[14]魏畅,傅红,郑俊超,等. QuRChERS-液质联用同步检测蘑菇中多菌灵等3种杀菌剂残留[J].食品工业,2016,16(11):189-195.
[15]张榕杰,张伟,马青青.超高效液相色谱-串联质谱法同时测定水果中9种杀菌剂的残留量[J].中国卫生检验杂志,2015,25(18):3080-3083.
[16]沈伟健,毛应民,吴斌.气相色谱-正化学源-质谱联用技术测定葡萄和葡萄酒中多种唑类杀菌剂的残留量[J].分析化学,2010,38(7):941-947.
[17] Matuszewski BK,Constanzer ML,Chavez-Eng CM. Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS[J]. Anal Chem,2003,75(13):3019-3030.
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