超高效液相色谱-四极杆飞行时间质谱法非靶向筛查西红柿中三唑类杀菌剂

doi:10.3724/SP.J.1123.2019.12020

色谱 ›› 2020, Vol. 38 ›› Issue (7): 805-816.DOI: 10.3724/SP.J.1123.2019.12020

超高效液相色谱-四极杆飞行时间质谱法非靶向筛查西红柿中三唑类杀菌剂

雷汝清¹^,²^,³, 牛宇敏²^,³, 郭巧珍²^,³, 邵兵²^,³, 丁晓静¹^,²^,³^,^*()

¹ 首都医科大学公共卫生学院, 北京 100069
² 北京市疾病预防控制中心, 食物中毒诊断溯源技术北京市重点实验室, 北京 100013
³ 北京市预防医学研究中心, 北京 100013

收稿日期:2019-12-16 出版日期:2020-07-08 发布日期:2020-12-10
通讯作者: 丁晓静
作者简介:丁晓静.Tel:64407087, E-mail:dxj666@aliyun.com
基金资助:
国家重点研发计划项目(2018YFC1602400);国家自然科学基金重点项目(U1736201)

Non-targeted screening of triazole fungicides in tomatoes by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry

LEI Ruqing¹^,²^,³, NIU Yumin²^,³, GUO Qiaozhen²^,³, SHAO Bing²^,³, DING Xiaojing¹^,²^,³^,^*()

¹ School of Public Health, Capital Medical University, Beijing 100069, China
² Beijing Center for Diseases Prevention and Control, Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing 100013, China
³ Beijing Center for Preventive Medicine Research, Beijing 100013, China

Received:2019-12-16 Online:2020-07-08 Published:2020-12-10
Contact: DING Xiaojing
Supported by:
National Key Research and Development Program(2018YFC1602400);National Natural Science Foundation of China(U1736201)

摘要/Abstract

摘要：

建立了超高效液相色谱-四极杆飞行时间质谱非靶向快速筛查西红柿中三唑类杀菌剂的方法。样品用乙腈提取、QuEChERS净化、BEH C₁₈（100 mm×2.1 mm，1.7 μm）色谱柱分离，以乙腈和水（均含0.1%（v/v）甲酸）为流动相进行梯度洗脱，采用四极杆飞行时间质谱仪进行检测。质谱离子源为电喷雾电离源，采集方式为正离子数据非依赖分析MS^E扫描模式。将19种三唑类杀菌剂按化学结构的不同分为8类。首先通过对8类典型三唑类杀菌剂中代表性的8种标准品的二级质谱图进行分析，总结出三唑类杀菌剂经碰撞诱导解离后产生的特征碎片离子和特征中性碎片丢失的质谱裂解规律，然后再利用另外11种三唑类杀菌剂标准品进行验证，并用于16份北京市售西红柿的非靶向筛查，在1份样品中筛查出烯唑醇。该方法快速、简便、准确率高，可为食品中三唑类杀菌剂残留的筛查提供参考。

关键词: 超高效液相色谱, 电喷雾电离, 飞行时间质谱, 三唑类杀菌剂, 裂解规律, 非靶向筛查

Abstract:

In order to cope with the differences in international trade regulations, it is necessary to establish a rapid non-targeted screening method for triazole fungicides in food. Therefore, a non-targeted method based on ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) was established for the rapid screening of triazole fungicides in tomatoes. Tomato samples were extracted with acetonitrile and then purified by QuEChERS. The purified solution was separated on a BEH C₁₈ column (100 mm×2.1 mm, 1.7 μm) using a gradient mobile phase consisting of acetonitrile and water (both containing 0.1% formic acid). Full information tandem mass spectrometry (MS^E) acquisition using electrospray ion source under positive ion mode was performed. The 19 triazole fungicides were divided into eight groups based on their structural differences. The secondary mass fragments of eight typical standards in the eight groups of triazole fungicides were analyzed, and then, the regularities of the characteristic fragment ions and neutral loss fragments produced by collision-induced dissociation of the triazole fungicides were summarized. The fragmentation regularity was further verified by the other 11 triazole fungicides. A total of 16 tomato samples collected from local supermarkets in Beijing were screened using this non-targeted method. Diniconazole was identified and confirmed in one sample, which demonstrated that the method could achieve rapid and accurate non-targeted screening of triazole fungicides in tomatoes. The proposed method is highly efficient, sensitive, and accurate, thus providing a reference for screening triazole fungicide residues in food.

Key words: ultra-high performance liquid chromatography (UPLC), electrospray ionization (ESI), time of flight mass spectrometry (TOF-MS), triazole fungicides, fragmentation regularity, non-targeted screening

雷汝清, 牛宇敏, 郭巧珍, 邵兵, 丁晓静. 超高效液相色谱-四极杆飞行时间质谱法非靶向筛查西红柿中三唑类杀菌剂[J]. 色谱, 2020, 38(7): 805-816.

LEI Ruqing, NIU Yumin, GUO Qiaozhen, SHAO Bing, DING Xiaojing. Non-targeted screening of triazole fungicides in tomatoes by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry[J]. Chinese Journal of Chromatography, 2020, 38(7): 805-816.

图/表 8

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No.	Compound	China/ (mg/kg)	United States/ (mg/kg)	European Union/ (mg/kg)
-: no clear limits of triazole fungicides in tomatoes.
1	tricyclazole (三环唑)	-	-	0.01
2	ametoctradin (唑嘧菌胺)	-	1.5	2
3	imibenconazole (亚胺唑)	-	0.6	2
4	flusilazole (氟硅唑)	0.2	-	0.01
5	penconazole (戊菌唑)	0.2	-	0.1
6	triadimefon (三唑酮)	1	-	0.01
7	diniconazole (烯唑醇)	-	-	0.01
8	uniconazole (烯效唑)	-	0.01	-
9	paclobutrazol (多效唑)	-	-	0.02
10	tebuconazole (戊唑醇)	0.2	1.3	0.9
11	cyproconazole (环丙唑醇)	-	-	0.05
12	flutriafol (粉唑醇)	-	1	0.8
13	tetraconazole (四氟醚唑)	-	0.3	0.1
14	myclobutanil (腈菌唑)	1	0.3	0.3
15	fenbuconazole (腈苯唑)	-	-	0.5
16	epoxiconazole (氟环唑)	-	-	0.05
17	bromuconazole (糠菌唑)	-	-	0.05
18	difenoconazole (苯醚甲环唑)	0.5	0.6	2
19	propiconazole (丙环唑)	3	3	3

No.	Compound	China/ (mg/kg)	United States/ (mg/kg)	European Union/ (mg/kg)
-: no clear limits of triazole fungicides in tomatoes.
1	tricyclazole (三环唑)	-	-	0.01
2	ametoctradin (唑嘧菌胺)	-	1.5	2
3	imibenconazole (亚胺唑)	-	0.6	2
4	flusilazole (氟硅唑)	0.2	-	0.01
5	penconazole (戊菌唑)	0.2	-	0.1
6	triadimefon (三唑酮)	1	-	0.01
7	diniconazole (烯唑醇)	-	-	0.01
8	uniconazole (烯效唑)	-	0.01	-
9	paclobutrazol (多效唑)	-	-	0.02
10	tebuconazole (戊唑醇)	0.2	1.3	0.9
11	cyproconazole (环丙唑醇)	-	-	0.05
12	flutriafol (粉唑醇)	-	1	0.8
13	tetraconazole (四氟醚唑)	-	0.3	0.1
14	myclobutanil (腈菌唑)	1	0.3	0.3
15	fenbuconazole (腈苯唑)	-	-	0.5
16	epoxiconazole (氟环唑)	-	-	0.05
17	bromuconazole (糠菌唑)	-	-	0.05
18	difenoconazole (苯醚甲环唑)	0.5	0.6	2
19	propiconazole (丙环唑)	3	3	3

No.	Compound	Formula	t/ min	Theoretical m/z	Full-scan		MS/MS
No.	Compound	Formula	t/ min	Theoretical m/z	Measured m/z	△mDa	Measured m/z	Formula	Structural feature
1	tricyclazole	C₉H₈N₃S	2.83	190.0433	190.0431	-0.2	163.0322	C₈H₇N₂S	[M+H-HCN]⁺
							136.0214	C₇H₆NS	[M+H-HCN-HCN]⁺
2	ametoctradin	C₁₅H₂₆N₅	4.31	276.2183	276.2182	-0.1	249.2082	C₁₄H₂₅N₄	[M+H-HCN]⁺
							149.0813	C₇H₉N₄	[M+H-HCN-C₇H₁₆]⁺
							176.0928	C₈H₁₀N₅	[M+H-C₇H₁₆]⁺
3	imibenconazole	C₁₇H₁₄C_l3N₄O	5.26	410.9999	410.9996	-0.3	341.9669	C₁₅H₁₁Cl₃NS	[M+H-C₂H₃N₃]⁺
							229.9591	C₉H₆Cl₂NS	[M+H-C₂H₃N₃-C₆H₅Cl]⁺
							125.0150	C₇H₆Cl	[M+H-C₂H₃N₃-C₈H₅Cl₂NS]⁺
							89.0384	C₇H₅	[M+H-C₂H₃N₃-C₈H₅Cl₂NS-HCl]⁺
4	flusilazole	C₁₆H₁₆F₂N₃Si	4.53	316.1076	316.1072	-0.4	247.0744	C₁₄H₁₃F₂Si	[M+H-C₂H₃N₃]⁺
							227.0682	C₁₄H₁₂FSi	[M+H-C₂H₃N₃-HF]⁺
							300.0767	C₁₅H₁₁F₂N₃Si	[M+H-CH₄]⁺
							219.0431	C₁₂H₉F₂Si	[M+H-CH₄-C₃H₃N₃]⁺
							123.0058	C₆H₃FSi	[M+H-CH₄-C₃H₃N₃-C₆H₅F]⁺
5	penconazole	C₁₃H₁₆Cl₂N₃	4.66	284.0716	284.0714	-0.2	215.0385	C₁₁H₁₃Cl₂	[M+H-C₂H₃N₃]⁺
							172.9919	C₈H₇Cl₂	[M+H-C₂H₃N₃-C₃H₆]⁺
							158.9762	C₇H₅Cl₂	[M+H-C₂H₃N₃-C₄H₈]⁺
							122.9996	C₇H₄Cl	[M+H-C₂H₃N₃-C₄H₈-HCl]⁺
							89.0384	C₇H₅	[M+H-C₂H₃N₃-C₄H₈-HCl+2H-HCl]⁺
10	tebuconazole	C₁₆H₂₂ClN₃O	4.55	308.1524	308.1521	-0.3	239.0545	C₁₄H₂₀ClO	[M+H-C₂H₃N₃]⁺
							181.0593	C₁₀H₁₀ClO	[M+H-C₂H₃N₃-C₄H₁₀]⁺
							151.0310	C₉H₈Cl	[M+H-C₂H₃N₃-C₄H₁₀-HCHO]⁺
							125.0153	C₇H₆Cl	[M+H-C₂H₃N₃-C₄H₁₀-HCHO-C₂H₂]⁺
							89.0384	C₇H₅	[M+H-C₂H₃N₃-C₄H₁₀-HCHO-C₂H₂-HCl]⁺
14	myclobutanil	C₁₅H₁₈ClN₄	4.38	289.1215	289.1212	-0.3	220.0885	C₁₃H₁₅ClN	[M+H-C₂H₃N₃]⁺
							178.0417	C₁₀H₉ClN	[M+H-C₂H₃N₃-C₃H₆]⁺
							151.0307	C₉H₈Cl	[M+H-C₂H₃N₃-C₃H₆-HCN]⁺
							125.0152	C₇H₆Cl	[M+H-C₂H₃N₃-C₂H₄-HCN-C₂H₂]⁺
							89.0383	C₇H₅	[M+H-C₂H₃N₃-C₂H₄-HCN-C₂H₂-HCl]⁺
							164.0261	C₉H₇ClN	[M+H-C₂H₃N₃-C₄H₈]⁺
							192.0571	C₁₁H₁₁ClN	[M+H-C₂H₃N₃-C₂H₄]⁺
17	bromuconazole	C₁₃H₁₃BrCl₂N₃O	4.31	375.9614	375.9612	-0.2	306.9289	C₁₁H₁₀BrCl₂O	[M+H-C₂H₃N₃]⁺
							227.0027	C₁₁H₉Cl₂O	[M+H-C₂H₃N₃-HBr]⁺
							199.0069	C₁₀H₉Cl₂	[M+H-C₂H₃N₃-HBr-CO]⁺
							158.9763	C₇H₅Cl₂	[M+H-C₂H₃N₃-HBr-CO-C₃H₄]⁺
							122.9996	C₇H₄Cl	[M+H-C₂H₃N₃-HBr-CO-C₃H₄-HCl]⁺
							144.9606	C₆H₃Cl₂	[M+H-C₂H₃N₃-HBr-CO-C₄H₆]⁺

No.	Compound	Formula	t/ min	Theoretical m/z	Full-scan		MS/MS
No.	Compound	Formula	t/ min	Theoretical m/z	Measured m/z	△mDa	Measured m/z	Formula	Structural feature
1	tricyclazole	C₉H₈N₃S	2.83	190.0433	190.0431	-0.2	163.0322	C₈H₇N₂S	[M+H-HCN]⁺
							136.0214	C₇H₆NS	[M+H-HCN-HCN]⁺
2	ametoctradin	C₁₅H₂₆N₅	4.31	276.2183	276.2182	-0.1	249.2082	C₁₄H₂₅N₄	[M+H-HCN]⁺
							149.0813	C₇H₉N₄	[M+H-HCN-C₇H₁₆]⁺
							176.0928	C₈H₁₀N₅	[M+H-C₇H₁₆]⁺
3	imibenconazole	C₁₇H₁₄C_l3N₄O	5.26	410.9999	410.9996	-0.3	341.9669	C₁₅H₁₁Cl₃NS	[M+H-C₂H₃N₃]⁺
							229.9591	C₉H₆Cl₂NS	[M+H-C₂H₃N₃-C₆H₅Cl]⁺
							125.0150	C₇H₆Cl	[M+H-C₂H₃N₃-C₈H₅Cl₂NS]⁺
							89.0384	C₇H₅	[M+H-C₂H₃N₃-C₈H₅Cl₂NS-HCl]⁺
4	flusilazole	C₁₆H₁₆F₂N₃Si	4.53	316.1076	316.1072	-0.4	247.0744	C₁₄H₁₃F₂Si	[M+H-C₂H₃N₃]⁺
							227.0682	C₁₄H₁₂FSi	[M+H-C₂H₃N₃-HF]⁺
							300.0767	C₁₅H₁₁F₂N₃Si	[M+H-CH₄]⁺
							219.0431	C₁₂H₉F₂Si	[M+H-CH₄-C₃H₃N₃]⁺
							123.0058	C₆H₃FSi	[M+H-CH₄-C₃H₃N₃-C₆H₅F]⁺
5	penconazole	C₁₃H₁₆Cl₂N₃	4.66	284.0716	284.0714	-0.2	215.0385	C₁₁H₁₃Cl₂	[M+H-C₂H₃N₃]⁺
							172.9919	C₈H₇Cl₂	[M+H-C₂H₃N₃-C₃H₆]⁺
							158.9762	C₇H₅Cl₂	[M+H-C₂H₃N₃-C₄H₈]⁺
							122.9996	C₇H₄Cl	[M+H-C₂H₃N₃-C₄H₈-HCl]⁺
							89.0384	C₇H₅	[M+H-C₂H₃N₃-C₄H₈-HCl+2H-HCl]⁺
10	tebuconazole	C₁₆H₂₂ClN₃O	4.55	308.1524	308.1521	-0.3	239.0545	C₁₄H₂₀ClO	[M+H-C₂H₃N₃]⁺
							181.0593	C₁₀H₁₀ClO	[M+H-C₂H₃N₃-C₄H₁₀]⁺
							151.0310	C₉H₈Cl	[M+H-C₂H₃N₃-C₄H₁₀-HCHO]⁺
							125.0153	C₇H₆Cl	[M+H-C₂H₃N₃-C₄H₁₀-HCHO-C₂H₂]⁺
							89.0384	C₇H₅	[M+H-C₂H₃N₃-C₄H₁₀-HCHO-C₂H₂-HCl]⁺
14	myclobutanil	C₁₅H₁₈ClN₄	4.38	289.1215	289.1212	-0.3	220.0885	C₁₃H₁₅ClN	[M+H-C₂H₃N₃]⁺
							178.0417	C₁₀H₉ClN	[M+H-C₂H₃N₃-C₃H₆]⁺
							151.0307	C₉H₈Cl	[M+H-C₂H₃N₃-C₃H₆-HCN]⁺
							125.0152	C₇H₆Cl	[M+H-C₂H₃N₃-C₂H₄-HCN-C₂H₂]⁺
							89.0383	C₇H₅	[M+H-C₂H₃N₃-C₂H₄-HCN-C₂H₂-HCl]⁺
							164.0261	C₉H₇ClN	[M+H-C₂H₃N₃-C₄H₈]⁺
							192.0571	C₁₁H₁₁ClN	[M+H-C₂H₃N₃-C₂H₄]⁺
17	bromuconazole	C₁₃H₁₃BrCl₂N₃O	4.31	375.9614	375.9612	-0.2	306.9289	C₁₁H₁₀BrCl₂O	[M+H-C₂H₃N₃]⁺
							227.0027	C₁₁H₉Cl₂O	[M+H-C₂H₃N₃-HBr]⁺
							199.0069	C₁₀H₉Cl₂	[M+H-C₂H₃N₃-HBr-CO]⁺
							158.9763	C₇H₅Cl₂	[M+H-C₂H₃N₃-HBr-CO-C₃H₄]⁺
							122.9996	C₇H₄Cl	[M+H-C₂H₃N₃-HBr-CO-C₃H₄-HCl]⁺
							144.9606	C₆H₃Cl₂	[M+H-C₂H₃N₃-HBr-CO-C₄H₆]⁺

No.	Compound	Formula	Theoretical m/z	Measured m/z	Common fragment ions (m/z)	Common neutral losses
6	triadimefon	C₁₄H₁₇ClN₃O₂	294.10038	294.10032	89.0386, 125.0153	C₂H₃N₃
7	diniconazole	C₁₅H₁₈Cl₂N₃O	326.08214	326.08293	70.0340, 89.0386, 122.9996, 125.0153	C₂H₃N₃, C₄H₈, C₇H₆, CO, HCl
8	uniconazole	C₁₅H₁₉ClN₃O	292.12112	292.12070	70.0340, 89.0386, 122.9996, 125.0153	C₂H₃N₃, C₄H₁₀, C₄H₈, CO
9	paclobutrazol	C₁₅H₂₁ClN₃O	294.13667	294.13656	70.0340, 89.0386, 125.0153	C₄H₁₀
11	cyproconazole	C₁₅H₁₉ClN₃O	292.12112	292.12152	70.0340, 89.0386, 125.0153	HCl
12	flutriafol	C₁₆H₁₄F₂N₃O	302.10994	302.10967	70.0340, 89.0386	C₂H₃N₃, C₃H₄, C₇H₆
13	tetraconazole	C₁₃H₁₂Cl₂F₄N₃O	372.02881	372.02846	70.0340, 89.0386, 122.9996, 125.0153	C₂H₃N₃, HCl
15	fenbuconazole	C₁₉H₁₈ClN₄	337.12145	337.12131	70.0340, 89.0386, 125.0153	C₂H₃N₃, HCN
16	epoxiconazole	C₁₇H₁₄ClFN₃O	330.08039	330.08014	70.0340, 89.0386, 125.0153	C₂H₃N₃, HCHO, HCl, HCN
18	difenoconazole	C₁₉H₁₈Cl₂N₃O₃	406.07197	406.07160	70.0340, 89.0386, 122.9996, 125.0153	C₂H₃N₃, C₄H₆, HCl
19	propiconazole	C₁₅H₁₈Cl₂N₃O₂	342.07706	342.07759	89.0386, 122.9996	C₂H₃N₃, HCl

超高效液相色谱-四极杆飞行时间质谱法非靶向筛查西红柿中三唑类杀菌剂

Non-targeted screening of triazole fungicides in tomatoes by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry

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Metrics

No.	Compound	Matrix effect/%
6	triadimefon	2.48
7	diniconazole	85.43
8	uniconazole	22.22
9	paclobutrazol	78.50
11	cyproconazole	72.31
12	flutriafol	61.27
13	tetraconazole	50.70
15	fenbuconazole	71.68
16	epoxiconazole	12.49
18	difenoconazole	64.42
19	propiconazole	76.77

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