Determination of DIMBOA Residues in Helicoverpa armigera by UPLC-MS/MS

doi:10.6048/j.issn.1001-4330.2021.10.010

Xinjiang Agricultural Sciences ›› 2021, Vol. 58 ›› Issue (10): 1846-1850.DOI: 10.6048/j.issn.1001-4330.2021.10.010

• Chemical Fertilizer and Pesticide Application Reduction for Cotton • Previous Articles Next Articles

Determination of DIMBOA Residues in Helicoverpa armigera by UPLC-MS/MS

Weizheng LI(), Zhongxiong NING, He LIANG, Wei LU()

Engineering Research Center of Cotton, Ministry of Education / Key Laboratory of the Pest Monitoring and Safety Control of Crops and Forests of the Universities of Xinjiang Uygur Autonomous Region /College of Agronomy, Xinjiang Agricultural University,Urumqi 830052, China

Received:2021-03-15 Online:2021-10-20 Published:2021-10-26
Correspondence author: Wei LU
Supported by:
National Natural Science Foundation of China(31660520);National Key R & D Program Project(2017YFD0201903);Special Fund for Cultivation of Scientific and Technological Innovation in Xinjiang Academy of Agricultural Sciences(xjkcpy-2020004)

UPLC-MS/MS测定棉铃虫体内丁布的残留量

李维政(), 宁忠雄, 梁赫, 路伟()

新疆农业大学农学院/棉花教育部工程研究中心/自治区农林有害生物监测与安全防控重点实验室,乌鲁木齐 830052

通讯作者: 路伟
作者简介:李维政(1997-),男,江苏宿迁人,硕士研究生,研究方向为棉花害虫绿色防控,(E-mail) leeweizheng@163.com
基金资助:
国家自然科学基金(31660520);国家重点研发计划(2017YFD0201903);新疆农科院科技创新重点培育专项(xjkcpy-2020004)

Abstract

Abstract:

【Objective】 To compared the effects of two pretreatment methods on the determination of DIMBOA in Helicoverpa armigera, and establish an UPLC-MS/MS method for the determination of DIMBOA in H. armigera. 【Methods】 The samples of H. armigera were extracted by methanol vortex oscillation and ultrasonic wave and the content of DIMBOA was determined by Waters UPLC-MS/MS (Xevo TQS mass spectrometry). The chromatographic column was BEH C18, the mobile phase was methanol- pure water (containing 0.5% glacial acetic acid) gradient elution, and the flow rate was 0.3 mL/min. 【Results】 At concentrations of 5 and 50 μg/L, the addition recovery rate of methanol ultrasonic extraction method was the best, the average addition recovery rates were 84.26% and 96.78%, respectively, and the limit of quantity was 5 μg/L. 【Conclusion】 The accuracy, precision and addition recovery of methanol ultrasonic extraction method meet the requirements of compound residue analysis.

Key words: DIMBOA; Helicoverpa armigera; UPLC-MS/MS; residue analysis

摘要：

【目的】对比2种前处理方法对丁布含量的影响,建立UPLC-MS/MS测定棉铃虫体内丁布含量的分析方法。【方法】棉铃虫样品经甲醇涡旋振荡、超声波提取,用Waters UPLC-MS/MS (Xevo TQS质谱)检测丁布的含量,BEH C₁₈色谱柱,流动相为甲醇-水(含0.5%的冰乙酸)梯度洗脱,流速0.3 mL/min。【结果】棉铃虫样品在低浓度5 μg/L、高浓度50 μg/L 2个添加水平下,甲醇超声提取法的添加回收率最佳,平均添加回收率分别为84.26%、96.78%,最低检测质量浓度为5 μg/L。【结论】该方法的准确度和精密度、添加回收率均符合化合物残留分析的要求。

关键词: 丁布, 棉铃虫, UPLC-MS/MS, 残留

CLC Number:

S435.622⁺3

Weizheng LI, Zhongxiong NING, He LIANG, Wei LU. Determination of DIMBOA Residues in Helicoverpa armigera by UPLC-MS/MS[J]. Xinjiang Agricultural Sciences, 2021, 58(10): 1846-1850.

李维政, 宁忠雄, 梁赫, 路伟. UPLC-MS/MS测定棉铃虫体内丁布的残留量[J]. 新疆农业科学, 2021, 58(10): 1846-1850.

Figures/Tables 5

References 12

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名称 Test cimpound	母离子 Parent ion (m/z)	子离子 Daughter ion (m/z)	锥孔电压 Cone voltage (V)	碰撞能 Impact energy (V)
丁布	212.0	166.0	40	10
DIMBOA		194.0	40	10

名称 Test cimpound	母离子 Parent ion (m/z)	子离子 Daughter ion (m/z)	锥孔电压 Cone voltage (V)	碰撞能 Impact energy (V)
丁布	212.0	166.0	40	10
DIMBOA		194.0	40	10

方法 Method	添加浓度 Fortified concentration (μg/L)	回收率 Recovery rate (%)						相对标准偏差 RSD (%)
方法 Method	添加浓度 Fortified concentration (μg/L)	1	2	3	4	5	平均值 Average value	相对标准偏差 RSD (%)
1	5	59.26	47.42	39.70	60.22	55.04	52.32	7.76
1	50	28.54	31.95	29.67	21.36	35.40	29.38	4.65
2	5	82.48	80.42	84.06	86.30	88.04	84.26	2.70
2	50	104.54	93.85	86.34	110.13	89.05	96.78	9.12

方法 Method	添加浓度 Fortified concentration (μg/L)	回收率 Recovery rate (%)						相对标准偏差 RSD (%)
方法 Method	添加浓度 Fortified concentration (μg/L)	1	2	3	4	5	平均值 Average value	相对标准偏差 RSD (%)
1	5	59.26	47.42	39.70	60.22	55.04	52.32	7.76
1	50	28.54	31.95	29.67	21.36	35.40	29.38	4.65
2	5	82.48	80.42	84.06	86.30	88.04	84.26	2.70
2	50	104.54	93.85	86.34	110.13	89.05	96.78	9.12

Determination of DIMBOA Residues in Helicoverpa armigera by UPLC-MS/MS

UPLC-MS/MS测定棉铃虫体内丁布的残留量

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References 12

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时间 Time (min)	流速 Flow rate (mL/min)	流动相A Mobile phase A (%)	流动相B Mobile phase B (%)
0	0.3	100	0
3	0.3	10	90
6	0.3	100	0

时间 Time (min)	流速 Flow rate (mL/min)	流动相A Mobile phase A (%)	流动相B Mobile phase B (%)
0	0.3	100	0
3	0.3	10	90
6	0.3	100	0