Objective To establish a QuEChERS isotope dilution ultra-high performance liquid chromatography-tandem mass spectrometry method for simultaneously determining eight pesticide residues,including cyromazine,in plant-based foods. Methods After weighing the sample,a mixed isotope internal standard was added,extracted by acetonitrile,sodium chloride and anhydrous sodium sulfate were added.After centrifugation,the supernatant was purified by ethylenediamine-N-propylsilanized silica gel (PSA),and determined by ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS),and quantified by internal standard method. Results The correlation coefficients of eight pesticides within the concentration range of 0.5~100 μg/L were 0.992 2 to 0.999 8,the detection limit was 0.000 1 to 0.002 mg/kg,and the quantitative limit was 0.0003 to 0.007 mg/kg.After adding three spiked concentrations of 0.002,0.02,and 0.12 mg/kg,the average recovery rate of this method was 86.5% to 110.0% with the relative standard deviation of 1.40% to 9.80%.This method was applied to detect 30 samples of commercially available fruits and vegetables,and all eight pesticides were detected,with detection rates of 3.33% to 33.33%,all of which did not exceed the standard.Some samples showed mixed residues of multiple pesticides. Conclusion This method can effectively avoid interference caused by matrix effects of different samples,and its accuracy,precision,and sensitivity all meet the requirements of detection standards.It has the characteristics of simplicity,stability,reliability,and ease of operation,and is suitable for the detection of batch samples.
Key words
QuEChERS /
Isotope-labeled internal standards /
UPLC-MS/MS /
Plant based food /
Pesticide residues
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References
[1] 董娇,曹宁阳,耿鑫.全自动固相萃取-高效液相色谱测定蔬菜中灭蝇胺残留[J].现代食品,2018(4):94-98.
[2] 宋卫国,饶钦雄,陈珊珊,等.同位素内标法检测灭蝇胺及其代谢物三聚氰胺在双孢蘑菇子实体和覆土中的残留[J].农药学学报,2018,20(3):363-369.
[3] 郑伟,王彬,吴亚维,等.不同杀菌剂对苹果白粉病病菌的室内毒力测定[J].江苏农业科学,2012,40(9):131-132.
[4] 张旭晟,高阳光,彭少杰.韭菜中农药腐霉利残留的膳食暴露风险评估[J].食品安全质量检测学报,2019,10(10):3114-3119.
[5] 崔晓岚,孟庆晓,毕扬,等.辣椒疫霉对烯酰吗啉的敏感性基线及室内抗药突变体研究[J].植物病理学报,2009,39(6):630-637.
[6] 庞怀林,杨建湘,杨剑波.杀菌剂烯酰吗啉的合成[C]//第三届湖北湖南植保农药学术研讨会论文集,武汉,2004:353-356.
[7] 李艳杰,喻歆茹,余婷,等.苯醚甲环唑在芹菜体系中的沉积与残留规律[J].现代农药,2020,19(2):37-40.
[8] Qin G,Chen Y,He F,et al.Risk assessment of fungicide pesticide residues in vegetables and fruits in the mid-western region of China[J].J Food Compos Anal,2021,95:103663.
[9] 安晶晶,刘新刚,董丰收,等.超高效液相色谱-串联质谱法测定土壤、蔬菜及水果中苯醚甲环唑和丙环唑残留[J].农药,2009,48(7):506-508.
[10] 李培培,陈敏,王军.QuEChERS-高效液相色谱法检测红葡萄酒中多菌灵和甲霜灵杀菌剂残留[J].食品与发酵工业,2015,41(1):202-206.
[11] 王艳春,赵旭东.蔬菜中农药多组分残留量的固相萃取-气相色谱测定法[J].环境与健康杂志,2010,27(5):445-447.
[12] 李芳,胡建民,李锋格,等.混合固相萃取柱净化-气相色谱质谱联用法快速测定果蔬中10种农药残留的研究[J].中国卫生检验杂志,2011,21(10):2416-2417+2420.
[13] 苗水,王柯,陆继伟,等.农药残留测定用新型混合型固相萃取小柱的开发[J].中国卫生检验杂志,2011,21(1):7-12.
[14] 崔春艳,张红医,吴兴强,等.分散固相萃取-液相色谱-串联质谱法测定谷物、蔬菜、水果中27种新型杀菌剂[J].色谱,2017,35(5):487-494.
[15] 邵华,金芬,杨锚,等.QuEChERS方法在我国农药残留分析中的应用与前景[J].农业质量标准,2007(S1):120-122.
[16] 杨春霞,卫平萍,余明池.QuEChERS-UPLC法测定水果中三氯杀螨醇和氰戊菊酯残留量[J].安徽预防医学杂志,2021,27(1):78-80.
[17] 黄芬,夏文斌,李雄伟,等.蔬菜中多种有机磷农药残留的固相萃取-气相色谱测定方法研究[J].实用预防医学,2017,24(5):627-629.
[18] 李志,焦彦朝,王兴宁.气相色谱-质谱联用法测定茶叶中21种农药残留[J].中国酿造,2019,38(3):181-186.
[19] 周迎春,姜太玲,熊贤坤,等.高效液相色谱法在蔬菜农药残留检测中的应用[J].农产品加工,2018(8):73-74+77.
[20] 马琳,黄兰淇,陈建波,等.超高效液相色谱-串联质谱法测定草莓中19种农药残留量[J].分析测试学报,2016,35(6):698-703.
[21] 王东斌,汪春明.QuEChERS-高效液相色谱-串联质谱法测定粮谷中啶磺草胺的残留[J].食品安全质量检测学报,2021,12(9):3799-3806.
[22] 黄何何,张缙,徐敦明,等.QuEChERS-高效液相色谱-串联质谱法同时测定水果中21种植物生长调节剂的残留量[J].色谱,2014,32(7):707-716.
[23] 杨路平,邵立君,王国玲,等.QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留[J].食品工业科技,2019,40(14):247-253.
[24] Chambers E,Wagrowski-Diehl DM,Lu Z,et al.Systematic and comprehensive strategy for reducing matrix effects in LC/MS/MS analyses[J].J Chromatogr B Analyt Technol Biomed Life Sci,2007,852(1/2):22-34.
[25] 许晓敏,李凌云,林桓,等.基质效应对液相色谱串联质谱分析农药残留的影响研究[J].农产品质量与安全,2019(6):11-15+20.
[26] Zhu Y,Liu X,Xu J,et al.Simultaneous determination of spirotetramat and its four metabolites in fruits and vegetables using a modified quick,easy,cheap,effective,rugged,and safe method and liquid chromatography/tandem mass spectrometry[J].J Chromatogr A,2013,1299:71-77.
[27] Duan Y,Guan N,Li P,et al.Monitoring and dietary exposure assessment of pesticide residues incowpea (Vigna unguiculata L.Walp) in Hainan,China[J].Food Contr,2016,59:250-255.