Determination of Imidacloprid and β-cypermethrin in Banana by UPLC-MS/MS

doi:10.3969/j.issn.1000-2561.2019.04.020

Abstract

Abstract:

A method was established for the simultaneous determination of imidacloprid and β-cypermethrin residues in bananas. The samples were extracted with 1% of acetic acid-acetonitrile, cleaned by PSA and GCB. Gradient elution separation was carried out with methanol and 2 mmol/L ammonium acetate solution as the mobile phase. The samples were determined using electrospray positive ionization (ESI ⁺) with multiple reaction monitoring (MRM) and then quantified by the matrix-matched external standard method. The results showed that the correlation coefficient r was > 0.9991, when the concentration ranged from 0.001 to 0.1 mg/L. The limit of detection (LOD) was 1 pg and the limit of quantification (LOQ) was 0.01 mg/kg. The recovery of imidacloprid and β-cypermethrin in banana was from 84.91% to 104.78% and the relative standard deviation (RSD) was from 1.23% to 9.69%. The method is simple, sensitive and reproducible for the determination of imidacloprid and β-cypermethrin residues in bananas.

Key words: banana, imidacloprid, β-cypermethrin;, UPLC-MS/MS

WANG Mimi,XIE Defang. Determination of Imidacloprid and β-cypermethrin in Banana by UPLC-MS/MS[J]. Chinese Journal of Tropical Crops, 2019, 40(4): 753-757.

Figures/Tables 6

References 20

[1]	张奇泓, 郭建辉, 蔡恩兴 , 等. 氯氰菊酯在香蕉、土壤上的残留动态及安全性评价[J]. 亚热带植物科学, 2013,42(3):245-248.
[2]	尹可锁, 杨韶松, 郑泗军 , 等. 吡虫啉不同施药方式防控香蕉蓟马的研究[J]. 中国南方果树, 2017,46(2):111-113.
[3]	曾鑫年, 林进添 . 黄胸蓟马对香蕉的危害及其防治[J]. 植物保护, 1998,24(6):15-17.
[4]	孟建玉, 张长禹, 陆宁 , 等. 贵州主要烟区烟蚜对吡虫啉的抗药性测定[J]. 江苏农业科学, 2015,43(4):162-164.
[5]	潘永波, 张艳玲 . 气相色谱法测定香蕉中的噻虫嗪和吡虫啉[J]. 农药, 2013,52(12):903-904.
[6]	蔡晓钰, 姜宇, 蒋宝南 , 等. 分散固相萃取-气相色谱法测定土壤中的高效氯氰菊酯残留[J]. 上海农业学报, 2018,34(1):101-105.
[7]	张雪辉, 杜雨倩, 徐芳 , 等. 高效液相色谱法检测蔬菜中的吡虫啉残留[J]. 现代食品科技, 2012,28(4):466-468, 482.
[8]	杨秋红, 刘欢, 李司棋 , 等. 高效液相色谱-三重四级杆质谱联用法测定水体、底泥和克氏原螯虾中的吡虫啉残留[J]. 农药, 2018,57(6):427-430.
[9]	冯义志, 潘金菊, 周力 , 等. 高效氯氰菊酯在韭菜中的残留消解动态及残留量[J]. 农药科学与管理, 2016,37(9):25-29.
[10]	周萍, 李英华, 胡福良 , 等. 高效液相色谱串联质谱法同时测定蜂王浆中氟胺氰菊酯、三唑醇和蝇毒磷残留[J]. 食品科学, 2013,34(18):180-184. DOI
[11]	刘冰洁, 贾春虹, 陈莉 , 等. QuEChERS-超高效液相色谱-串联质谱法测定吡虫啉在花椰菜和土壤中的残留[J]. 食品安全质量检测学报, 2018,9(6):1254-1260.
[12]	李国烈, 杜鑫, 苏旭 , 等. 超高效液相色谱-串联质谱方法测定桑葚中吡虫啉和啶虫脒残留量[J]. 农药科学与管理, 2018,39(1):41-46, 52.
[13]	李菊颖, 郭欣妍, 何健 , 等. 玉米粉中吡虫啉、三唑酮、乙草胺与异丙甲草胺的QuEChERS/高效液相色谱-串联质谱快速检测[J]. 分析测试学报, 2017,36(6):783-787.
[14]	李俊芳, 杜光明, 李德强 , 等. 苹果中痕量吡虫啉农药的固相萃取及高效液相色谱-串联质谱分析[J]. 农药, 2016,55(3):194-197, 213.
[15]	苏敏, 李世雨, 李锋格 , 等. 超高效液相色谱-串联质谱法快速检测番茄酱中吡虫啉等6种农药残留[J]. 色谱, 2011,29(11):1070-1075. DOI
[16]	Kim Y A, Abd El-Aty A M, Rahman M M , et al. Method development, matrix effect, and risk assessment of 49 multiclass pesticides in kiwifruit using liquid chromatography coupled to tandem mass spectrometry[J]. Journal of Chromatography B, 2018,1076:130-138. DOI URL
[17]	Faraji M, Noorbakhsh R, Shafieyan H , et al. Determination of acetamiprid, imidacloprid, and spirotetramat and their relevant metabolites in pistachio using modified QuEChERS combined with liquid chromatography-tandem mass spectrometry[J]. Food Chemistry, 2018,240:634-641. DOI URL
[18]	程功, 刘娜, 田宏哲 , 等. QuEChERS-高效液相色谱-串联质谱法测定丙炔氟草胺在食品和环境中的残留及土壤中的消解动态[J]. 农药学学报, 2018,20(1):75-82.
[19]	吴燕梅, 邓华阳, 杨钦沾 , 等. 优化的QuEChERS/超高液相色谱-串联质谱法测定鲜茶叶中21种氨基甲酸酯类农药残留[J]. 化学研究与应用, 2018,30(3):437-443.
[20]	孙利东, 许秀丽, 袁飞 , 等. 高效液相色谱-串联质谱法测定牛奶和鸡肉中4种激素本底值[J]. 食品科学, 2017,38(22):291-297.

化合物 Compound	保留时间 Retention time/min	离子对 Ion pair / (m?z^-1)	去簇电压 Decluster voltage/V	碰撞能量 Collision energy/V
吡虫啉 Imidacloprid	0.96	256.0/209.0^*	60.50	23.29
吡虫啉 Imidacloprid	0.96	256.0/175.1	60.50	24.39
高效氯氰菊酯 β-cypermethrin	2.90	433.0/191.0^*	70.98	19.96
高效氯氰菊酯 β-cypermethrin	2.90	433.0/119.0	70.98	20.14

化合物 Compound	保留时间 Retention time/min	离子对 Ion pair / (m?z^-1)	去簇电压 Decluster voltage/V	碰撞能量 Collision energy/V
吡虫啉 Imidacloprid	0.96	256.0/209.0^*	60.50	23.29
吡虫啉 Imidacloprid	0.96	256.0/175.1	60.50	24.39
高效氯氰菊酯 β-cypermethrin	2.90	433.0/191.0^*	70.98	19.96
高效氯氰菊酯 β-cypermethrin	2.90	433.0/119.0	70.98	20.14

提取剂 Extracting agent	吡虫啉 Imidacloprid		高效氯氰菊酯 β-cypermethrin
提取剂 Extracting agent	蕉肉 Banana pulp	全蕉 Whole banana	蕉肉 Banana pulp	全蕉 Whole banana
乙腈 Acetonitrile	74.34±0.22	77.74±0.21	93.73±5.39	106.77±6.40
0.1%甲酸乙腈 0.1% formic acid acetonitrile	76.57±0.68	77.08±0.85	101.24±3.20	106.35±3.76
1%甲酸乙腈 1% formic acid acetonitrile	110.06±2.16	111.01±2.73	93.40±3.86	95.05±3.42
0.1%乙酸乙腈 0.1% acetonitrile acetate	80.60±2.37	82.83±1.03	86.22±3.69	99.83±1.61
1%乙酸乙腈 1% acetonitrile acetate	89.59±0.88	100.31±1.96	89.77±3.96	100.41±9.70

提取剂 Extracting agent	吡虫啉 Imidacloprid		高效氯氰菊酯 β-cypermethrin
提取剂 Extracting agent	蕉肉 Banana pulp	全蕉 Whole banana	蕉肉 Banana pulp	全蕉 Whole banana
乙腈 Acetonitrile	74.34±0.22	77.74±0.21	93.73±5.39	106.77±6.40
0.1%甲酸乙腈 0.1% formic acid acetonitrile	76.57±0.68	77.08±0.85	101.24±3.20	106.35±3.76
1%甲酸乙腈 1% formic acid acetonitrile	110.06±2.16	111.01±2.73	93.40±3.86	95.05±3.42
0.1%乙酸乙腈 0.1% acetonitrile acetate	80.60±2.37	82.83±1.03	86.22±3.69	99.83±1.61
1%乙酸乙腈 1% acetonitrile acetate	89.59±0.88	100.31±1.96	89.77±3.96	100.41±9.70

化合物 Compound	基质 Matrix	PSA/mg			GCB/mg
化合物 Compound	基质 Matrix	100	200	300	10	50	100
吡虫啉 Imidacloprid	蕉肉 Banana pulp	93.27	98.15	98.46	93.77	95.99	93.83
吡虫啉 Imidacloprid	全蕉 Whole banana	93.70	95.99	96.30	94.44	94.44	94.04
高效氯氰菊酯 β-cypermethrin	蕉肉 Banana pulp	89.22	93.09	88.53	88.69	93.77	98.94
高效氯氰菊酯 β-cypermethrin	全蕉 Whole banana	88.15	93.85	83.14	91.12	96.51	99.62