UPLC-MS/MS测定棉铃虫体内丁布的残留量

doi:10.6048/j.issn.1001-4330.2021.10.010

新疆农业科学 ›› 2021, Vol. 58 ›› Issue (10): 1846-1850.DOI: 10.6048/j.issn.1001-4330.2021.10.010

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

收稿日期:2021-03-15 出版日期:2021-10-20 发布日期:2021-10-26
通信作者: 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)

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)

摘要/Abstract

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

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

中图分类号:

S435.622⁺3

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.

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.

图/表 5

参考文献 12

[1]	李晓辉, 刘青, 扶蓉, 等. 丁布(DIMBOA)研究进展[J]. 安徽农业科学, 2007,(19):5680-5681,5690.
	LI Xiaohui, LIU Qing, FU Rong, et al. Research Advance on DIMBOA[J]. Anhui Agricultural Sciences, 2007,(19):5680-5681,5690.
[2]	吴艳兵, 田发军, 赵欢欢, 等. 丁布的生物活性研究进展[J]. 植物保护, 2014, 40(5):8-13.
	WU Yanbing, TIAN Fajun, ZHAO Huanhuan, et al. Research Progress on the Biological Activity of DOMBOA[J]. Plant Protection, 2014, 40(5):8-13.
[3]	刘小红, 刘西莉, 李健强. 高效液相色谱/质谱法测定4个玉米品种幼苗中丁布含量[J]. 分析化学, 2004,(12):1641-1644.
	LIU Xiaohong, LIU Xili, LI Jianqiang. Determination of Difference of 2, 4-Dihydroxy-7-Methoxy-2H-1, 4- Benzoxazin-3(4H)-one Contents in Seedling of Four Maize Cultivars by High Performance Liquid Chromatography and Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2004,(12):1641-1644.
[4]	宋鹏飞, 王甜甜, 毛培, 等. 不同玉米品种丁布含量及其与抗螟性的关系[J]. 华中昆虫研究, 2012, (8):58-63.
	SONG Pengfei, WANG Tiantian, MAO Pei, et al. Relationship Between Butbutyl Content of Different Maize Varieties and Its Resistance to Borer[J]. Entomological Research in Central China, 2012, (8):58-63.
[5]	李晓辉, 黄京华, 王艳, 等. 高效液相色谱法测定不同玉米品种黄化苗丁布含量[J]. 玉米科学, 2008, (2):46-49.
	LI Xiaohui, HUANG Jinhua, WANG Yan, et al. The Methods of HPLC Detected the Content of Etiolated Seeding DIMBOA among Different Maize[J]. Journal of Maize Sciences, 2008,(2):46-49.
[6]	Wu K, Feng H, Guo Y. Evaluation of maize as a refuge for management of resistance to Bt cotton by Helicoverpa armigera (Hübner) in the Yellow River cotton-farming region of China[J]. Crop Protection, 2004, 23(6):523-530. DOI URL
[7]	吴莉莉, 王登元, 吕昭智, 等. 转基因抗虫棉田棉铃虫庇护所的建立和评价[J]. 新疆农业科学, 2011, 48(2):334-339.
	WU Lili, WANG Dengyuan, LÜ Zhaozhi, et al. Establishment and Evaluation of Refuge for Helicoverpa armigera Hübner of Bt Cotton Fields[J]. Xinjiang Agricultural Sciences, 2011, 48(2):334-339.
[8]	Glauser G, Marti G, Villard N, et al. Induction and detoxification of maize 1, 4-benzoxazin-3-ones by insect herbivores[J]. Plant Journal, 2011, 68(5):901-911. DOI URL
[9]	张晓影, 王朋, 周斌. 冬小麦幼苗生长和化感物质对CO₂和O₃浓度升高的响应[J]. 应用生态学报, 2013, 24(10):2843-2849. PMID
	ZHANG Xiaoying, WANG Peng, ZHOU Bin. Responses of winter wheat seedling growth and allelochemical content to elevated CO₂ and O₃ concentrations[J]. Chinese Journal of Applied Ecology, 2013, 24(10):2843-2849. PMID
[10]	Larsen E, Cheistensen L P. Simple method for large scale isolation of the cyclic arylhdroxamic acids DIMBOA from maize (Zea mays L)[J]. J Agric Food Chem, 2000, 48(6):2556-2558. DOI URL
[11]	刘保川, 陈巨莲, 倪汉祥, 等. 丁布的分离、纯化和结构鉴定及其对麦长管蚜生长、发育的影响[J]. 应用与环境生物学报, 2002, 8(1):71-74.
	LIU Baochuan, CHEN Julian, NI Hanxiang, et al. Isolation, purification and structural identification of DIMBOA and ITS resistance to English grain aphin, Stiobionavenae(F.)[J]. Chinese Journal of Applied & Environmental Biology, 2002, 8(1):71-74.
[12]	Li J, Liu X G, Dong F S, et al. A Simple Method for the Isolation and Purification of 2,4-Dihydroxy-7-Methoxy-2H-1,4-Benzoxazin-3(4H)-One (DIMBOA) from Maize (Zea mays L.) Seedlings[J]. Journal of Integrative Agriculture, 2013, 12(1):95-102. DOI URL

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

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UPLC-MS/MS测定棉铃虫体内丁布的残留量

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

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参考文献 12

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Metrics

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