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表 1 22 种磺胺标准品 Table 1 The standard compounds of 22 sulfonamides 结构式 Structure NR1HSNOR2HO 磺胺名称 Sulfonamides R1 R2 CAS pKa 分子式 Formula 分子量 MW 磺胺胍 Sulfaguanidine H HCNHNH2 57-67-0 11.3 C7H10N4O2S 214.24 磺胺 Sulfanilamide H H 63-74-1 10.4 C6H8N2O2S 172.20 磺胺嘧啶 Sulfadiazine H NN 68-35-9 6.5 C10H10N4O2S 250.28 磺胺二甲异嘧啶 Sulfisomidine H NNCH3CH3 515-64-0 7.4 C12H14N4O2S 278.33 磺胺醋酰 Sulfacetamide H HCOCH3 144-80-9 5.4 C8H10N2O3S 214.24 磺胺噻唑 Sulfathiazole H NS 72-14-0 7.2 C9H9N3O2S2 255.32 磺胺吡啶 Sulfapyridine H N 144-83-2 8.4 C11H11N3O2S 249.29 磺胺甲基嘧啶 Sulfamerazine H NNCH3 127-79-7 7.0 C11H12N4O2S 264.30 磺胺对甲氧嘧啶 Sulfameter H NNOCH3 651-06-9 6.7 C11H12N4O3S 280.30 磺胺二甲噁唑 Sulfamoxole H NOCH3CH3 729-99-7 7.2 C11H13N3O3S 267.30 磺胺二甲嘧啶 Sulfamethazine H NNCH3CH3 57-68-1 7.4 C12H14N4O2S 278.33 磺胺甲噻二唑 Sulfamethizole H NNSCH3 144-82-1 5.5 C9H10N4O2S2 270.33 磺胺甲氧哒嗪 Sulfamethoxypyridazine H NNOCH3 80-35-3 6.7 C11H12N4O3S 280.30 琥珀酰磺胺噻唑 Succinylsulfathiazole CHOH2CH2CCOOH NS 116-43-8-C13H13N3O5S2 355.39 磺胺氯哒嗪 Sulfachloropyridazine H NNCl 80-32-0 5.9 C10H9ClN4O2S284.72 磺胺甲基异噁唑 Sulfamethoxazole H NOCH3 723-46-6 6.0 C10H11N3O3S 253.28 磺胺间甲氧嘧啶 Sulfamonomethoxine H NNOCH3 1220-83-36.5 C11H12N4O3S 280.30 磺胺邻二甲氧嘧啶 Sulfadoxine H NNOCH3H3CO 2447-57-65.9 C12H14N4O4S 310.33 磺胺二甲异噁唑 Sulfisoxazole H ONCH3H3C 127-69-5 5.0 C11H13N3O3S 267.30 磺胺间二甲氧嘧啶 Sulfadimethoxine H NNOCH3OCH3 122-11-2 6.3 C12H14N4O4S 310.33 磺胺喹噁啉 Sulfaquinoxaline H NN 59-40-5 5.5 C14H12N4O2S 300.34 磺胺硝苯 Sulfanitran CHH3CO NO2 122-16-7 14.5 C14H13N3O5S 335.34 2.2 色谱条件色谱条件 Waters ACQUITY UPLC BEH C18柱(1.7 m,2.1 mm50 mm);流动相:甲醇(A)和0.1%甲酸水溶液(B),梯度洗脱程序:0 2.6 min,5%A 16%A;2.6 3.8 min,16%A 22%A;3.8 4.8 min,22%A 25%A;4.8 6.6 min,25%A;6.6 7.0 min,25%A 55%A;7.0 9.2 min,55%A 95%A;9.2 10.0 min,95%A,10.0 11.0 min,95%A 8%A;流速0.2 mL/min;柱温30;样品室温度20;进样量5 L。2.3 质谱条件质谱条件 电喷雾离子源;正离子扫描;毛细管电压3.5 kV;射频透镜电压0.0 V;离子源温度120;去溶剂气温度350;去溶剂气流量500 L/h;锥孔气流量50 L/h;光电倍增器电压650 V;碰撞气体为氩气,碰撞气压3.210-3 mbar;多反应监测(MRM)模式检测,22种磺胺的质谱分析参数见表2。表2 22种磺胺的质谱分析参数 Table 2 MS parameters for 22 sulfonamides analysis 磺胺名称 Sulfonamides 保留时间 Retention time(min)监测离子对 Monitoring ion pairs(m/z)锥孔电压 Cone voltage(V)碰撞能量 Collision Energy(eV)215.8/108.6 22 23 磺胺胍 Sulfaguanidine 0.89 215.8/156.9 22 15 173.2/91.4 15 18 磺胺 Sulfanilamide 0.99 173.2/155.9 15 7 215.2/91.5 30 20 磺胺嘧啶 Sulfadiazine 1.84 215.2/156.0 30 17 251.1/107.7 25 23 磺胺二甲异嘧啶 Sulfisomidine 2.43 251.1/156.0 25 15 279.2/123.8 15 22 磺胺醋酰 Sulfacetamide 2.67 279.2/186.1 15 10 256.2/107.6 25 23 磺胺噻唑 Sulfathiazole 3.00 256.2/156.0 25 15 250.2/156.0 27 15 磺胺吡啶 Sulfapyridine 3.22 250.2/184.2 27 17 265.2/156.0 27 17 磺胺甲基嘧啶 Sulfamerazine 3.52 265.2/172.0 27 15 281.2/156.0 25 18 磺胺对甲氧嘧啶 Sulfameter 4.44 281.2/215.2 25 18 268.2/112.7 23 23 磺胺二甲噁唑 Sulfamoxole 4.52 268.2/156.0 23 15 279.2/156.0 25 17 磺胺二甲嘧啶 Sulfamethazine 4.59 279.2/186.1 25 15 271.2/107.7 26 17 磺胺甲噻二唑 Sulfamethizole 4.70 271.2/156.0 26 17 281.2/107.7 27 27 磺胺甲氧哒嗪 Sulfamethoxypyridazine 5.05 281.2/156.0 27 17 琥珀酰磺胺噻唑 5.32 356.1/156.1 32 23 Succinylsulfathiazole 356.1/256.2 32 17 285.2/107.7 25 25 磺胺氯哒嗪 Sulfachloropyridazine 5.44 285.2/156.0 25 15 254.2/107.7 25 22 磺胺甲基异噁唑 Sulfamethoxazole 5.78 254.2/156.0 25 17 281.1/156.0 28 17 磺胺间甲氧嘧啶 Sulfamonomethoxine 5.89 281.1/215.2 28 15 311.2/107.7 30 30 磺胺邻二甲氧嘧啶 Sulfadoxine 6.21 311.2/156.0 30 18 268.2/112.7 23 15 磺胺二甲异噁唑 Sulfisoxazole 6.50 268.2/156.0 23 13 311.2/107.8 25 25 磺胺间二甲氧嘧啶 Sulfadimethoxine 8.05 311.2/156.1 25 15 301.2/107.8 35 27 磺胺喹噁啉 Sulfaquinoxaline 8.12 301.2/156.1 35 20 336.2/156.1 25 13 磺胺硝苯 Sulfanitran 8.49 336.2/294.3 25 10
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