杂质吸附型净化结合超高效液相色谱-串联质谱法同时测定谷物和动物饲料中37种霉菌毒素

doi:10.3724/SP.J.1123.2019.12013

色谱 ›› 2020, Vol. 38 ›› Issue (7): 817-825.DOI: 10.3724/SP.J.1123.2019.12013

杂质吸附型净化结合超高效液相色谱-串联质谱法同时测定谷物和动物饲料中37种霉菌毒素

王瑞国¹, 郭丽丽¹, 王培龙¹, 苏晓鸥¹^,^*(), 宋志超², 林刚³, 朱荣华³

¹ 中国农业科学院农业质量标准与检测技术研究所, 农业部农产品质量安全研究重点实验室, 北京 100081
² 河南省兽药饲料监察所, 河南郑州 450008
³ 奥特奇生物制品(中国)有限公司, 北京 100600

收稿日期:2019-12-07 出版日期:2020-07-08 发布日期:2020-12-10
通讯作者: 苏晓鸥
作者简介:苏晓鸥.Tel:82106307, E-mail:suxiaoou@caas.cn
基金资助:
国家重点研发计划项目(2017YFC1600300);国家现代农业产业技术体系(CARS-35)

Simultaneous determination of 37 mycotoxins in grain and animal feed by impurity adsorption purification coupled with ultra-performance liquid chromatography-tandem mass spectrometry

WANG Ruiguo¹, GUO Lili¹, WANG Peilong¹, SU Xiao'ou¹^,^*(), SONG Zhichao², LIN Gang³, ZHU Ronghua³

¹ Institute of Quality Standards and Testing Technology for Agricultural Products, Chinese Academy of Agricultural Science, Key Laboratory of Agrifood Safety and Quality, Ministry of Agriculture, Beijing 100081, China
² Henan Institute of Veterinary Drug and Feed Control, Zhengzhou 450008, China
³ Alltech Biological Products(China)Co., Ltd, Beijing 100600, China

Received:2019-12-07 Online:2020-07-08 Published:2020-12-10
Contact: SU Xiao'ou
Supported by:
National Key R & D Program of China(2017YFC1600300);China Agriculture Research System(CARS-35)

摘要/Abstract

摘要：

建立了谷物和动物饲料中霉菌毒素的高效、快速前处理方法，可同时提取和净化样品中37种理化性质差异较大的霉菌毒素，并采用超高效液相色谱-串联质谱（UPLC-MS/MS）进行定性和定量分析。样品粉碎处理后，经84%（体积分数，下同）乙腈水（含0.1%甲酸）溶液振荡提取20 min，MLJ-1杂质吸附型固相萃取柱净化。目标物在BEH RP18色谱柱上分离，以0.1 mmol/L乙酸铵溶液（含0.1%甲酸）和甲醇溶液（含0.1%甲酸）作为流动相进行梯度洗脱，质谱采用电喷雾正、负离子模式和多反应监测模式进行定性和定量分析。结果表明，本方法可在1 min内完成样品净化处理，15 min内完成37种目标化合物的分离分析。37种目标物在各自线性范围内线性关系良好，基质匹配标准曲线的相关系数均大于0.98。除伏马毒素外的所有目标化合物在4个添加水平下的回收率介于80%~120%之间，相对标准偏差（RSD）<20%（n=5），方法定量限为2~40 μg/kg，能够满足《饲料卫生标准》判定要求。该方法操作简单、快速、准确，适合谷物和动物饲料中多种霉菌毒素同步筛查和确证检测。

关键词: 杂质吸附, 固相萃取, 超高效液相色谱-串联质谱法, 霉菌毒素, 谷物, 饲料

Abstract:

A rapid method based on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC–MS/MS) was developed for the simultaneous determination of 37 mycotoxins having various physicochemical properties in grain and animal feed samples. The 37 analytes were extracted from ground samples with acetonitrile-water-formic acid (84:15.9:0.1, v/v/v) by 20 min vibration, and purified using a commercial MLJ-1 pass-through solid-phase extraction (SPE) clean-up cartridge. The analytes were then separated on a reversed-phase BEH RP18 column by a gradient elution program with 0.1 mmol/L ammonium acetate (containing 0.1% (v/v) formic acid) aqueous solution and 0.1% (v/v) formic acid methanol solution as mobile phases. The separated analytes were detected by MS/MS in the multiple reaction monitoring (MRM) mode via ESI+/- ionization. The results showed that the purification was completed in 1 min and that the 37 analytes could be separated on the chromatographic column in 15 min. The 37 mycotoxins showed a linear relationship within their respective linear ranges, and the correlation coefficients of the matrix-matched calibration curves were greater than 0.98. The average recoveries at four spiked levels (limit of quantification (LOQ), LOQ×5, LOQ×10, LOQ×25) for all the targets except fumonisins ranged from 80% to 120%, with the relative standard deviations (RSDs) lower than 20% (n=6). The limits of quantification (LOQs) for all the analytes were between 2 and 40 μg/kg. The proposed method is simple, fast, and accurate, thus being suitable for detecting multiple mycotoxins in grain and animal feed samples.

Key words: impurity adsorption, solid phase extraction (SPE), ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), mycotoxins, grain, feed

王瑞国, 郭丽丽, 王培龙, 苏晓鸥, 宋志超, 林刚, 朱荣华. 杂质吸附型净化结合超高效液相色谱-串联质谱法同时测定谷物和动物饲料中37种霉菌毒素[J]. 色谱, 2020, 38(7): 817-825.

WANG Ruiguo, GUO Lili, WANG Peilong, SU Xiao'ou, SONG Zhichao, LIN Gang, ZHU Ronghua. Simultaneous determination of 37 mycotoxins in grain and animal feed by impurity adsorption purification coupled with ultra-performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2020, 38(7): 817-825.

图/表 7

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Group	No.	Compound	Retention time/min	Adduct	Precursor ion (m/z)	Product ions (m/z)	CV/V	CE/eV
*Quantification ion.
A	1	aflatoxin B₁ (黄曲霉毒素B₁)	8.25	[M+H]⁺	313.1	284.9^*, 241.0	46	26, 40
	2	aflatoxin B₂ (黄曲霉毒素B₂)	7.92	[M+H]⁺	315.2	287.1^*, 259.0	46	30, 32
	3	aflatoxin G₁ (黄曲霉毒素G₁)	7.73	[M+H]⁺	329.1	242.9^*, 200.0	42	28, 42
	4	aflatoxin G₂ (黄曲霉毒素G₂)	7.39	[M+H]⁺	331.1	189.0^*, 245.0	48	43, 34
	5	sterigmatocystin (杂色曲霉素)	10.81	[M+H]⁺	324.8	310.0^*, 280.8	45	26, 46
B	6	ochratoxin A (赭曲霉毒素A)	10.61	[M+H]⁺	404.1	238.9^*, 220.9	32	28, 40
	7	ochratoxin B (赭曲霉毒素B)	9.83	[M+H]⁺	370.2	204.9^*, 102.8	25	25, 54
	8	T-2 toxin (T-2毒素)	9.63	[M+NH₄]⁺	484.2	185.1^*, 305.3	24	25, 18
	9	T-2 triol (T-2三醇)	8.34	[M+Na]⁺	405.2	303.1^*, 125.0	62	14, 16
	10	HT-2 toxin (HT-2毒素)	9.03	[M+NH₄]⁺	442.2	263.2^*, 245.1	30	10, 10
	11	lysergol (麦角醇)	4.32	[M+H]+	254.8	197.0^*, 44.0	15	24, 15
	12	ergocornine (麦角柯宁碱)	7.72	[M+H]⁺	562.2	208.0^*, 223.1	36	48, 40
	13	zearalenone (玉米赤霉烯酮)	10.83	[M-H]^-	317.2	131.0^*, 175.1	48	35, 30
	14	α-zearalenol (α-玉米赤霉烯醇)	10.96	[M-H]^-	319.0	275.1^*, 301.1	44	33, 30
	15	β-zearalenol (β-玉米赤霉烯醇)	10.34	[M-H]^-	319.0	275.1^*, 301.1	42	32, 28
	16	zearalanone (玉米赤霉酮)	10.70	[M-H]^-	319.0	275.1^*, 301.1	43	28, 34
	17	α-zearalanol (α-玉米赤霉醇)	10.69	[M-H]^-	321.0	277.2^*, 303.2	42	26, 26
	18	β-zearalanol (β-玉米赤霉醇)	10.11	[M-H]^-	321.0	277.2^*, 303.2	40	28, 32
C	19	deoxynivalenol (脱氧雪腐镰刀菌烯醇)	4.38	[M+H]⁺	296.9	249.1^*, 231.1	15	10, 15
	20	15-acetyldeoxynivalenol	6.75	[M+H]⁺	338.6	137.0^*, 321.0	25	22, 15
		(15-乙酰基脱氧雪腐镰刀菌烯醇)
	21	3-acetyldeoxynivalenol	6.75	[M+H]⁺	339.0	231.0^*, 203.1	28	16, 22
		(3-乙酰基脱氧雪腐镰刀菌烯醇)
	22	fumonisin B₁ (伏马毒素B₁)	8.69	[M+H]⁺	722.2	352.3^*, 334.3	50	36, 40
	23	fumonisin B₂ (伏马毒素B₂)	9.49	[M+H]⁺	706.4	336.5^*, 354.5	40	40, 35
	24	fumonisin B₃ (伏马毒素B₃)	9.14	[M+H]⁺	706.4	336.5^*, 354.5	40	40, 34
	25	fusarenon X (镰刀菌烯酮-X)	5.65	[M+H]⁺	355.1	247.1^*, 175.1	24	14, 22
	26	diacetoxyscirpenol (蛇形菌素)	8.07	[M+NH₄]⁺	384.2	307.2^*, 105.0	25	15, 30
	27	neosolaniol (新茄病镰刀菌烯醇)	6.09	[M+NH₄]⁺	400.2	185.0^*, 215.1	24	25, 20
	28	tentoxin (腾毒素)	9.32	[M+H]⁺	415.2	312.2^*, 256.1	66	20, 28
	29	patulin (展青霉素)	2.30	[M+H]⁺	155.0	71.0^*, 81.0	30	10, 10
	30	glotoxin (胶霉毒素)	8.30	[M+H]⁺	327.4	263.1^*, 245.1	26	14, 22
	31	verruculogen (疣孢青霉原)	10.71	[M+Na]⁺	534.0	392.1^*, 435.2	30	18, 20
	32	penitrem A (青霉震颤素A)	11.78	[M+H]⁺	634.3	558.3^*, 616.3	22	18, 10
	33	penicillic acid (青霉酸)	5.46	[M+H]⁺	171.0	97.0^*, 82.0	20	17, 25
	34	mycophenolic acid (霉酚酸)	9.69	[M+H]⁺	320.9	207.0^*, 159.0	25	26, 32
	35	roquefortine C (娄地青霉素C)	7.89	[M+H]⁺	389.9	193.0^*, 108.2	40	30, 42
	36	citreoviridin (黄绿青霉素)	10.38	[M+H]⁺	403.1	297.0^*, 285.0	35	18, 20
	37	wortmannin (渥曼青霉素)	8.36	[M+H]⁺	429.0	355.1^*, 313.1	18	12, 18

Group	No.	Compound	Retention time/min	Adduct	Precursor ion (m/z)	Product ions (m/z)	CV/V	CE/eV
*Quantification ion.
A	1	aflatoxin B₁ (黄曲霉毒素B₁)	8.25	[M+H]⁺	313.1	284.9^*, 241.0	46	26, 40
	2	aflatoxin B₂ (黄曲霉毒素B₂)	7.92	[M+H]⁺	315.2	287.1^*, 259.0	46	30, 32
	3	aflatoxin G₁ (黄曲霉毒素G₁)	7.73	[M+H]⁺	329.1	242.9^*, 200.0	42	28, 42
	4	aflatoxin G₂ (黄曲霉毒素G₂)	7.39	[M+H]⁺	331.1	189.0^*, 245.0	48	43, 34
	5	sterigmatocystin (杂色曲霉素)	10.81	[M+H]⁺	324.8	310.0^*, 280.8	45	26, 46
B	6	ochratoxin A (赭曲霉毒素A)	10.61	[M+H]⁺	404.1	238.9^*, 220.9	32	28, 40
	7	ochratoxin B (赭曲霉毒素B)	9.83	[M+H]⁺	370.2	204.9^*, 102.8	25	25, 54
	8	T-2 toxin (T-2毒素)	9.63	[M+NH₄]⁺	484.2	185.1^*, 305.3	24	25, 18
	9	T-2 triol (T-2三醇)	8.34	[M+Na]⁺	405.2	303.1^*, 125.0	62	14, 16
	10	HT-2 toxin (HT-2毒素)	9.03	[M+NH₄]⁺	442.2	263.2^*, 245.1	30	10, 10
	11	lysergol (麦角醇)	4.32	[M+H]+	254.8	197.0^*, 44.0	15	24, 15
	12	ergocornine (麦角柯宁碱)	7.72	[M+H]⁺	562.2	208.0^*, 223.1	36	48, 40
	13	zearalenone (玉米赤霉烯酮)	10.83	[M-H]^-	317.2	131.0^*, 175.1	48	35, 30
	14	α-zearalenol (α-玉米赤霉烯醇)	10.96	[M-H]^-	319.0	275.1^*, 301.1	44	33, 30
	15	β-zearalenol (β-玉米赤霉烯醇)	10.34	[M-H]^-	319.0	275.1^*, 301.1	42	32, 28
	16	zearalanone (玉米赤霉酮)	10.70	[M-H]^-	319.0	275.1^*, 301.1	43	28, 34
	17	α-zearalanol (α-玉米赤霉醇)	10.69	[M-H]^-	321.0	277.2^*, 303.2	42	26, 26
	18	β-zearalanol (β-玉米赤霉醇)	10.11	[M-H]^-	321.0	277.2^*, 303.2	40	28, 32
C	19	deoxynivalenol (脱氧雪腐镰刀菌烯醇)	4.38	[M+H]⁺	296.9	249.1^*, 231.1	15	10, 15
	20	15-acetyldeoxynivalenol	6.75	[M+H]⁺	338.6	137.0^*, 321.0	25	22, 15
		(15-乙酰基脱氧雪腐镰刀菌烯醇)
	21	3-acetyldeoxynivalenol	6.75	[M+H]⁺	339.0	231.0^*, 203.1	28	16, 22
		(3-乙酰基脱氧雪腐镰刀菌烯醇)
	22	fumonisin B₁ (伏马毒素B₁)	8.69	[M+H]⁺	722.2	352.3^*, 334.3	50	36, 40
	23	fumonisin B₂ (伏马毒素B₂)	9.49	[M+H]⁺	706.4	336.5^*, 354.5	40	40, 35
	24	fumonisin B₃ (伏马毒素B₃)	9.14	[M+H]⁺	706.4	336.5^*, 354.5	40	40, 34
	25	fusarenon X (镰刀菌烯酮-X)	5.65	[M+H]⁺	355.1	247.1^*, 175.1	24	14, 22
	26	diacetoxyscirpenol (蛇形菌素)	8.07	[M+NH₄]⁺	384.2	307.2^*, 105.0	25	15, 30
	27	neosolaniol (新茄病镰刀菌烯醇)	6.09	[M+NH₄]⁺	400.2	185.0^*, 215.1	24	25, 20
	28	tentoxin (腾毒素)	9.32	[M+H]⁺	415.2	312.2^*, 256.1	66	20, 28
	29	patulin (展青霉素)	2.30	[M+H]⁺	155.0	71.0^*, 81.0	30	10, 10
	30	glotoxin (胶霉毒素)	8.30	[M+H]⁺	327.4	263.1^*, 245.1	26	14, 22
	31	verruculogen (疣孢青霉原)	10.71	[M+Na]⁺	534.0	392.1^*, 435.2	30	18, 20
	32	penitrem A (青霉震颤素A)	11.78	[M+H]⁺	634.3	558.3^*, 616.3	22	18, 10
	33	penicillic acid (青霉酸)	5.46	[M+H]⁺	171.0	97.0^*, 82.0	20	17, 25
	34	mycophenolic acid (霉酚酸)	9.69	[M+H]⁺	320.9	207.0^*, 159.0	25	26, 32
	35	roquefortine C (娄地青霉素C)	7.89	[M+H]⁺	389.9	193.0^*, 108.2	40	30, 42
	36	citreoviridin (黄绿青霉素)	10.38	[M+H]⁺	403.1	297.0^*, 285.0	35	18, 20
	37	wortmannin (渥曼青霉素)	8.36	[M+H]⁺	429.0	355.1^*, 313.1	18	12, 18

No.	Matrix effects							LOQ/ (μg/kg)	Range/ (μg/L)
No.	Corn	Wheat flour	Cotton meal	Soybean meal	Pig concentrated feed	Pig compound feed	Cattle concentrate supplement	LOQ/ (μg/kg)	Range/ (μg/L)
Nos. are consistent with those of mycotoxins inTable 1.
1	0.89	1.03	0.61	0.87	0.98	0.88	1.02	2	0.5-25
2	0.90	1.00	0.76	0.62	1.21	0.81	1.70	2	0.5-25
3	0.95	1.01	0.83	0.99	0.87	0.88	0.65	2	0.5-25
4	0.95	1.04	0.87	0.98	1.21	0.90	0.46	2	0.5-25
5	0.72	0.76	0.59	0.76	0.97	0.72	0.88	2	0.5-25
6	0.94	0.92	0.87	1.06	1.01	0.95	1.01	20	5-250
7	0.98	0.94	0.98	1.18	1.31	0.91	1.11	20	5-250
8	0.87	0.82	0.77	0.83	0.91	0.68	0.82	20	5-250
9	1.13	0.96	0.38	0.97	0.18	0.82	0.04	20	5-250
10	1.01	0.98	0.63	0.32	0.84	0.38	0.78	20	5-250
11	0.89	0.94	0.76	1.44	2.07	0.96	1.94	20	5-250
12	0.36	0.37	0.22	0.28	0.39	0.68	0.33	20	5-250
13	0.82	0.93	0.81	0.99	0.94	1.18	1.12	20	5-250
14	0.87	1.14	0.82	1.03	1.15	1.57	1.29	20	5-250
15	0.85	0.97	0.78	1.03	0.67	1.22	1.05	20	5-250
16	0.81	0.94	0.80	1.01	1.03	1.11	1.21	20	5-250
17	0.87	1.10	0.89	1.12	0.86	1.28	1.18	20	5-250
18	0.86	1.07	0.77	1.07	1.06	1.15	0.97	20	5-250
19	0.81	1.03	0.67	1.00	1.02	0.75	0.70	40	10-500
20	0.79	0.87	0.62	0.79	0.87	0.40	0.66	40	10-500
21	0.79	0.90	0.61	0.84	0.89	0.46	0.66	40	10-500
22	2.36	1.47	2.54	1.13	1.00	3.84	1.17	40	10-500
23	1.72	1.78	1.76	0.94	1.03	2.14	1.04	40	10-500
24	1.31	1.71	2.06	1.06	1.16	3.55	1.37	40	10-500
25	1.02	1.03	0.84	0.96	1.05	0.84	0.59	40	10-500
26	0.99	0.97	0.86	0.97	1.51	0.89	1.66	40	10-500
27	1.04	1.00	0.94	1.02	1.19	0.91	0.65	40	10-500
28	0.91	0.96	0.79	0.96	1.15	0.84	0.91	40	10-500
29	0.89	0.98	1.00	0.89	1.02	0.84	0.76	40	10-500
30	0.46	0.50	0.27	0.22	1.16	0.30	1.20	40	10-500
31	0.84	0.90	0.56	1.27	0.26	1.09	1.08	40	10-500
32	0.59	0.66	0.53	0.70	0.76	0.77	0.80	40	10-500
33	1.00	1.03	0.98	1.04	1.83	0.90	0.96	40	10-500
34	1.04	0.93	0.91	1.06	1.63	0.98	1.57	40	10-500
35	0.62	0.87	0.59	0.78	0.54	0.71	0.49	40	10-500
36	0.83	0.89	0.71	1.24	1.61	0.97	1.21	40	10-500
37	0.73	0.80	0.22	0.64	0.47	0.58	0.64	40	10-500

No.	Matrix effects							LOQ/ (μg/kg)	Range/ (μg/L)
No.	Corn	Wheat flour	Cotton meal	Soybean meal	Pig concentrated feed	Pig compound feed	Cattle concentrate supplement	LOQ/ (μg/kg)	Range/ (μg/L)
Nos. are consistent with those of mycotoxins inTable 1.
1	0.89	1.03	0.61	0.87	0.98	0.88	1.02	2	0.5-25
2	0.90	1.00	0.76	0.62	1.21	0.81	1.70	2	0.5-25
3	0.95	1.01	0.83	0.99	0.87	0.88	0.65	2	0.5-25
4	0.95	1.04	0.87	0.98	1.21	0.90	0.46	2	0.5-25
5	0.72	0.76	0.59	0.76	0.97	0.72	0.88	2	0.5-25
6	0.94	0.92	0.87	1.06	1.01	0.95	1.01	20	5-250
7	0.98	0.94	0.98	1.18	1.31	0.91	1.11	20	5-250
8	0.87	0.82	0.77	0.83	0.91	0.68	0.82	20	5-250
9	1.13	0.96	0.38	0.97	0.18	0.82	0.04	20	5-250
10	1.01	0.98	0.63	0.32	0.84	0.38	0.78	20	5-250
11	0.89	0.94	0.76	1.44	2.07	0.96	1.94	20	5-250
12	0.36	0.37	0.22	0.28	0.39	0.68	0.33	20	5-250
13	0.82	0.93	0.81	0.99	0.94	1.18	1.12	20	5-250
14	0.87	1.14	0.82	1.03	1.15	1.57	1.29	20	5-250
15	0.85	0.97	0.78	1.03	0.67	1.22	1.05	20	5-250
16	0.81	0.94	0.80	1.01	1.03	1.11	1.21	20	5-250
17	0.87	1.10	0.89	1.12	0.86	1.28	1.18	20	5-250
18	0.86	1.07	0.77	1.07	1.06	1.15	0.97	20	5-250
19	0.81	1.03	0.67	1.00	1.02	0.75	0.70	40	10-500
20	0.79	0.87	0.62	0.79	0.87	0.40	0.66	40	10-500
21	0.79	0.90	0.61	0.84	0.89	0.46	0.66	40	10-500
22	2.36	1.47	2.54	1.13	1.00	3.84	1.17	40	10-500
23	1.72	1.78	1.76	0.94	1.03	2.14	1.04	40	10-500
24	1.31	1.71	2.06	1.06	1.16	3.55	1.37	40	10-500
25	1.02	1.03	0.84	0.96	1.05	0.84	0.59	40	10-500
26	0.99	0.97	0.86	0.97	1.51	0.89	1.66	40	10-500
27	1.04	1.00	0.94	1.02	1.19	0.91	0.65	40	10-500
28	0.91	0.96	0.79	0.96	1.15	0.84	0.91	40	10-500
29	0.89	0.98	1.00	0.89	1.02	0.84	0.76	40	10-500
30	0.46	0.50	0.27	0.22	1.16	0.30	1.20	40	10-500
31	0.84	0.90	0.56	1.27	0.26	1.09	1.08	40	10-500
32	0.59	0.66	0.53	0.70	0.76	0.77	0.80	40	10-500
33	1.00	1.03	0.98	1.04	1.83	0.90	0.96	40	10-500
34	1.04	0.93	0.91	1.06	1.63	0.98	1.57	40	10-500
35	0.62	0.87	0.59	0.78	0.54	0.71	0.49	40	10-500
36	0.83	0.89	0.71	1.24	1.61	0.97	1.21	40	10-500
37	0.73	0.80	0.22	0.64	0.47	0.58	0.64	40	10-500

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杂质吸附型净化结合超高效液相色谱-串联质谱法同时测定谷物和动物饲料中37种霉菌毒素

Simultaneous determination of 37 mycotoxins in grain and animal feed by impurity adsorption purification coupled with ultra-performance liquid chromatography-tandem mass spectrometry

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