Determination of 17 sulfonamides in infant formula by accelerated extraction and ultra-high performance liquid chromatography/mass spectrometry

doi:10.3969/j.issn.1004-1524.2023.01.19

Acta Agriculturae Zhejiangensis ›› 2023, Vol. 35 ›› Issue (1): 175-183.DOI: 10.3969/j.issn.1004-1524.2023.01.19

• Quality and Safety of Agricultural Products • Previous Articles Next Articles

Determination of 17 sulfonamides in infant formula by accelerated extraction and ultra-high performance liquid chromatography/mass spectrometry

JI Xiaofeng¹(), WANG Xiaoli¹, LYU Wentao¹, ZHOU Zhongjing², WU YUxiao³, YANG Hua¹^,^*()

1. Institute of Agro-Product Safety and Nutrition, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China
2. State Key Laboratory for Managing Biotic and Chemical Threats to the Quality and Safety of Agro-Products, Hangzhou 310021, China
3. College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310014, China

Received:2021-08-19 Online:2023-01-25 Published:2023-02-21

Abstract

Abstract:

A method for the determination of 17 sulfonamides residues in infant formula by accelerated solvent extraction (ASE) and ultra-high performance liquid chromatography/mass spectrometry (UHPLC-MS/MS) was developed. The linearity, sensitivity, recovery rate and matrix effect of the method were verified. Meanwhile, the screening analysis for 17 sulfonamides in infant formula collected from the market was carried out. The results showed that the linearity of sulfonamides were in the range of 0.5-100 μg·kg^-1, and the correlation coefficient was greater than 0. 998, the recoveries were 75.3%-103.6%, the relative standard deviation was less than 11.0%, the matrix effect was 0.4-1.0, the detection limit for sulfonamides in infant formula was 0.1-3.0 μg·kg^-1, and the limit of quantification (LOQ) was 0.3-10 μg·kg^-1. The developed method has the merits for convenient extraction, high sensitivity and accuracy, and the method can simultaneously determine 17 sulfonamides residues in infant formula.

Key words: accelerated solvent extraction (ASE), ultra-high performance liquid chromatography/mass spectrometry (HPLC-MS/MS), infant formula, sulfonamides

CLC Number:

TS252.51

JI Xiaofeng, WANG Xiaoli, LYU Wentao, ZHOU Zhongjing, WU YUxiao, YANG Hua. Determination of 17 sulfonamides in infant formula by accelerated extraction and ultra-high performance liquid chromatography/mass spectrometry[J]. Acta Agriculturae Zhejiangensis, 2023, 35(1): 175-183.

Figures/Tables 6

References 17

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编号 Number	化合物 Compound	CAS号 CAS number
1	磺胺醋酰Sulfacetamide	144-80-9
2	磺胺嘧啶Sulfadiazine	68-35-9
3	磺胺噻唑Sulfathiazloe	72-14-0
4	磺胺吡啶Sulfapyridine	144-83-2
5	磺胺甲基嘧啶Sulfamerazine	127-79-7
6	磺胺对甲氧嘧啶Sulfameter	651-06-9
7	磺胺甲噻二唑Sulfamethizole	144-82-1
8	磺胺二甲嘧啶Sulfamethazine	57-68-1
9	磺胺甲氧哒嗪Sulfamethoxypyridazine	80-35-3
10	磺胺甲噁唑Sulfamethoxazole	723-46-6
11	磺胺间甲氧嘧啶Sulfamonomethoxine	1220-83-3
12	磺胺邻二甲氧嘧啶Sulfadoxine	2447-57-6
13	磺胺二甲异噁唑Sulfamethoxazole	723-46-6
14	苯甲酰磺胺Sulfabenzamide	127-71-9
15	磺胺苯吡唑Sulfaphenazolum	526-08-9
16	磺胺间二甲氧嘧啶Sulfadimethoxypyrimidine	155-91-9
17	磺胺喹噁啉Sulfaquinoxaline	59-40-5

编号 Number	化合物 Compound	CAS号 CAS number
1	磺胺醋酰Sulfacetamide	144-80-9
2	磺胺嘧啶Sulfadiazine	68-35-9
3	磺胺噻唑Sulfathiazloe	72-14-0
4	磺胺吡啶Sulfapyridine	144-83-2
5	磺胺甲基嘧啶Sulfamerazine	127-79-7
6	磺胺对甲氧嘧啶Sulfameter	651-06-9
7	磺胺甲噻二唑Sulfamethizole	144-82-1
8	磺胺二甲嘧啶Sulfamethazine	57-68-1
9	磺胺甲氧哒嗪Sulfamethoxypyridazine	80-35-3
10	磺胺甲噁唑Sulfamethoxazole	723-46-6
11	磺胺间甲氧嘧啶Sulfamonomethoxine	1220-83-3
12	磺胺邻二甲氧嘧啶Sulfadoxine	2447-57-6
13	磺胺二甲异噁唑Sulfamethoxazole	723-46-6
14	苯甲酰磺胺Sulfabenzamide	127-71-9
15	磺胺苯吡唑Sulfaphenazolum	526-08-9
16	磺胺间二甲氧嘧啶Sulfadimethoxypyrimidine	155-91-9
17	磺胺喹噁啉Sulfaquinoxaline	59-40-5

化合物名称 Compound name	母离子 Precursor ion(m/z)	子离子 Sub ion (m/z)	去簇电压 Declustering voltage/eV	碰撞能量 Collision energy/eV	保留时间 Retention time/min
磺胺醋酰Sulfacetamide	215.0	156.0^*	52	15	2.18
		108.0	52	29
磺胺嘧啶Sulfadiazine	251.1	156.0^*	63	22	2.45
		108.1	63	34
磺胺噻唑Sulfathiazole	256.1	156.1^*	60	22	2.67
		108.1	60	35
磺胺吡啶Sulfapyridine	250.1	156.0^*	65	23	2.79
		184.1	65	23
磺胺甲基嘧啶Sulfamerazine	265.1	156.1^*	73	24	2.94
		172.0	73	24
磺胺对甲氧嘧啶Sulfameter	281.0	156.1^*	90	27	3.39
		108.1	90	42
磺胺甲噻二唑Sulfamethothiadiazole	271.0	156.1^*	65	21	3.87
		108.0	65	36
磺胺二甲嘧啶Sulfamethazine	279.1	186.0^*	75	25	3.35
		124.1	75	35
磺胺甲氧哒嗪Sulfamethoxypyridazine	281.0	156.0^*	75	25	3.38
		126.1	75	27
磺胺甲噁唑Sulfamethoxazole	254.1	156.0^*	70	23	3.88
		108.0	70	32
磺胺间甲氧嘧啶Sulfamonomethoxine	281.1	156.0^*	75	25	3.37
		126.2	75	30
磺胺邻二甲氧嘧啶Sulfadoxine	311.0	156.0^*	80	26	3.87
		108.0	80	37
磺胺二甲异噁唑Sulfisoxazole	268.1	156.0^*	80	26	4.01
		113.1	82	23
苯甲酰磺胺Sulfabenzamide	277.1	156.0^*	60	19	4.18
		108.1	60	32
磺胺苯吡唑Sulfaphenazolum	315.0	156.0^*	84	29	4.30
		108.1	60	32
磺胺间二甲氧嘧啶Sulfamethoxine	311.0	156.18^*	80	31	4.26
		108.1	80	38
磺胺喹噁啉Sulfaquinoxaline	301.1	156.1^*	80	24	5.08
		108.0	80	36

化合物名称 Compound name	母离子 Precursor ion(m/z)	子离子 Sub ion (m/z)	去簇电压 Declustering voltage/eV	碰撞能量 Collision energy/eV	保留时间 Retention time/min
磺胺醋酰Sulfacetamide	215.0	156.0^*	52	15	2.18
		108.0	52	29
磺胺嘧啶Sulfadiazine	251.1	156.0^*	63	22	2.45
		108.1	63	34
磺胺噻唑Sulfathiazole	256.1	156.1^*	60	22	2.67
		108.1	60	35
磺胺吡啶Sulfapyridine	250.1	156.0^*	65	23	2.79
		184.1	65	23
磺胺甲基嘧啶Sulfamerazine	265.1	156.1^*	73	24	2.94
		172.0	73	24
磺胺对甲氧嘧啶Sulfameter	281.0	156.1^*	90	27	3.39
		108.1	90	42
磺胺甲噻二唑Sulfamethothiadiazole	271.0	156.1^*	65	21	3.87
		108.0	65	36
磺胺二甲嘧啶Sulfamethazine	279.1	186.0^*	75	25	3.35
		124.1	75	35
磺胺甲氧哒嗪Sulfamethoxypyridazine	281.0	156.0^*	75	25	3.38
		126.1	75	27
磺胺甲噁唑Sulfamethoxazole	254.1	156.0^*	70	23	3.88
		108.0	70	32
磺胺间甲氧嘧啶Sulfamonomethoxine	281.1	156.0^*	75	25	3.37
		126.2	75	30
磺胺邻二甲氧嘧啶Sulfadoxine	311.0	156.0^*	80	26	3.87
		108.0	80	37
磺胺二甲异噁唑Sulfisoxazole	268.1	156.0^*	80	26	4.01
		113.1	82	23
苯甲酰磺胺Sulfabenzamide	277.1	156.0^*	60	19	4.18
		108.1	60	32
磺胺苯吡唑Sulfaphenazolum	315.0	156.0^*	84	29	4.30
		108.1	60	32
磺胺间二甲氧嘧啶Sulfamethoxine	311.0	156.18^*	80	31	4.26
		108.1	80	38
磺胺喹噁啉Sulfaquinoxaline	301.1	156.1^*	80	24	5.08
		108.0	80	36

化合物 Analytes	线性方程 Linear equation (y=ax+b)	决定系数 Coefficient of determination	斜率比值 Slope ratio	线性范围 Linear range/ (μg·L^-1)	LOD/ (μg· kg^-1)	LOQ/ (μg· kg^-1)
磺胺醋酰 Sulfacetamide	y=18 761x+7 174.6 y=45 155x-3 368.8	1.000 0 0.999 2	0.4	2.0~100	1.7	5.6
磺胺嘧啶 Sulfadiazine	y=42 579x+34 764 y=103 097x-31 951	0.999 2 0.999 9	0.4	2.0~100	0.4	1.1
磺胺噻唑 Sulfathiazole	y=44 461x-58 830 y=85 664x-60 190	0.996 8 0.999 3	0.5	2.0~100	0.5	1.7
磺胺吡啶 Sulfapyridine	y=52 323x-27 360 y=82 882x-33 480	0.999 9 0.999 9	0.6	2.0~100	0.6	2.0
磺胺甲基嘧啶 Sulfamerazine	y=47 332x-32 171 y=70 193x+6 914.8	0.998 5 0.998 4	0.7	3.0~100	0.7	2.2
磺胺对甲氧嘧啶 Sulfameter	y=43 180x-19 057 y=44 636x-25 855	0.999 8 0.998 4	1.0	1.0~100	0.2	0.6
磺胺甲噻二唑 Sulfamethothiadiazole	y=34 150x +4 228.1 y=62 481x+2 898	1.000 0 0.999 4	0.5	3.0~100	0.7	2.4
磺胺二甲嘧啶 Sulfamethazine	y=62 692x-35 071 y=95 526x-38 990	0.998 5 0.999 9	0.7	2.0~100	0.4	1.2
磺胺甲氧哒嗪 Sulfamethoxypyridazine	y=41 430x+26 833 y=45 946x +15 427	0.998 0 0.999 9	0.9	0.5~100	0.2	0.5
磺胺甲噁唑 Sulfamethoxazole	y=38 557x-8 886.5 y=78 617x+67 423	0.999 9 0.999 7	0.5	2.0~100	0.5	1.5
磺胺间甲氧嘧啶 Sulfamonomethoxine	y=41 816x-2 479.8 y=52 204x-47 066	0.999 8 0.999 7	0.8	0.5~100	0.2	0.4
磺胺邻二甲氧嘧啶 Sulfadoxine	y=91 379x-13 557 y=123 159x +81 006	1.000 0 0.999 5	0.4	0.5~100	0.2	0.4
磺胺二甲异噁唑 Sulfisoxazole	y=51 289x-10 742 y=101 514x+36 754	0.999 9 0.999 9	0.5	0.5~100	0.1	0.3
苯甲酰磺胺 Sulfabenzamide	y=47 283x-35 803 y=103 187x-310.6	0.998 0 1.000 0	0.5	1.0~100	0.2	0.7
磺胺苯吡唑 Sulfaphenazolum	y=17 396x+2 658.6 y=35 490x+56 214	0.999 7 0.999 0	0.5	10~100	3.0	10
磺胺间二甲氧嘧啶 Sulfamethoxine	y=100 765x-65 256 y=162 365x+23 126	0.999 7 0.999 9	0.6	1.0~100	0.2	0.6
磺胺喹噁啉 Sulfaquinoxaline	y=51 283x+34 423 y=85 486x+30 977	0.999 3 0.999 5	0.6	1.0~100	0.2	0.7

Determination of 17 sulfonamides in infant formula by accelerated extraction and ultra-high performance liquid chromatography/mass spectrometry

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References 17

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化合物 Analytes	回收率Recoveries(RSD)
化合物 Analytes	10 μg·kg^-1	20 μg·kg^-1	50 μg·kg^-1
磺胺醋酰Sulfacetamide	81.0(3.4)	85.9(5.6)	88.1(4.8)
磺胺嘧啶Sulfadiazine	75.3(7.4)	76.6(6.3)	77.8(7.1)
磺胺噻唑Sulfathiazole	92.7(1.7)	88.1(0.7)	89.2(3.4)
磺胺吡啶Sulfapyridine	83.1(6.0)	80.0(4.5)	80.0(9.1)
磺胺甲基嘧啶Sulfamerazine	103.6(7.8)	99.0(4.3)	91.2(7.8)
磺胺对甲氧嘧啶Sulfameter	76.7(3.3)	78.9(10.4)	84.4(9.1)
磺胺甲噻二唑Sulfamethothiadiazole	84.4(3.7)	86.9(5.8)	80.0(4.2)
磺胺二甲嘧啶Sulfamethazine	92.5(9.4)	84.3(6.0)	88.7(8.2)
磺胺甲氧哒嗪Sulfamethoxypyridazine	90.8(10.6)	96.6(11.0)	88.8(5.5)
磺胺甲噁唑Sulfamethoxazole	78.8(2.4)	77.5(4.1)	76.2(7.9)
磺胺间甲氧嘧啶Sulfamonomethoxine	84.7(2.7)	76.5(3.8)	79.8(9.1)
磺胺邻二甲氧嘧啶Sulfadoxine	75.7(3.6)	78.8(5.6)	76.6(7.8)
磺胺二甲异噁唑Sulfisoxazole	93.1(4.5)	89.9(8.6)	94.8(3.2)
苯甲酰磺胺Sulfabenzamide	78.8(9.0)	79.9(10.2)	81.3(9.7)
磺胺苯吡唑Sulfaphenazolum	79.8(1.5)	83.2(0.5)	78.5(7.2)
磺胺间二甲氧嘧啶Sulfamethoxine	87.5(2.9)	89.0(5.6)	82.1(8.7)
磺胺喹噁啉Sulfaquinoxaline	75.8(4.3)	79.8(6.6)	75.7(8.7)

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