色谱 ›› 2022, Vol. 40 ›› Issue (12): 1076-1086.DOI: 10.3724/SP.J.1123.2022.03039
收稿日期:
2022-03-25
出版日期:
2022-12-08
发布日期:
2022-11-29
通讯作者:
罗瑞涟
LUO Ruilian1,*(), WU Zhengshuang1, LIANG Chiqiong1, LUO Liting2
Received:
2022-03-25
Online:
2022-12-08
Published:
2022-11-29
Contact:
LUO Ruilian
摘要:
生产婴幼儿辅助食品的原辅料中常常含有鱼类、肉类、肝类等动物性组织,存在兽药残留的风险,为了更加全面地对这类产品进行安全监管,研究并开发了同时检测婴幼儿辅助食品中6大类(喹诺酮类、磺胺类、大环内酯类、硝基咪唑类、氯霉素类和抗病毒类)50种抗生素和抗病毒类兽药残留的超高效液相色谱-三重四极杆质谱法(UPLC-MS/MS)。样品采用酸化乙腈超声提取,提取液经新型的脂质增强型Captiva EMR-Lipid固相萃取柱净化,浓缩复溶后采用流动相乙腈和0.1%(v/v)甲酸水溶液,经C18柱梯度洗脱分离,电喷雾多反应监测(MRM)模式检测,基质匹配外标法定量。结果显示,该方法50种兽药在0.5~50 μg/L范围内线性关系较好,相关系数均不低于0.995,方法检出限为0.03~0.70 μg/kg,定量限为0.09~2.33 μg/kg。50种化合物在不同基质中,添加5和50 μg/kg两个加标水平进行试验,平均回收率为64.37%~119.3%,相对标准偏差均小于15%。将该方法应用于14份国产和6份进口的婴幼儿辅助食品检测,结果显示,1份进口肉类婴幼儿辅助食品中检出磺胺喹噁啉、磺胺二甲嘧啶和替米考星。该方法简单快速,灵敏度和准确度高,样品量消耗少,适用于婴幼儿辅助食品中多种兽药残留的检测。
中图分类号:
罗瑞涟, 吴正双, 梁炽琼, 罗丽婷. 超高效液相色谱-串联质谱法检测婴幼儿辅助食品中多种兽药残留[J]. 色谱, 2022, 40(12): 1076-1086.
LUO Ruilian, WU Zhengshuang, LIANG Chiqiong, LUO Liting. Determination of multi-veterinary drug residues in complementary foods for infants and young children by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2022, 40(12): 1076-1086.
Type | Compound | tR/min | Qualitative ions (m/z) | Declustering potential/V | Collision energies/eV |
---|---|---|---|---|---|
Fluoroquinolones | orbiflixacin (奥比沙星) | 3.41 | 396.1/352.1*, 396.1/295.1 | 150 | 27, 34 |
pipemidic acid (吡哌酸) | 2.36 | 304.2/217.2*, 304.2/189.1 | 150 | 32, 42 | |
danofloxacin (丹诺沙星) | 3.23 | 358.1/340.1*, 358.1/283.1 | 140 | 35, 34 | |
oxolinic acid (噁喹酸) | 4.06 | 262.1/244.1*, 262.1/216.1 | 130 | 29, 40 | |
enrofloxacin (恩诺沙星) | 3.33 | 360.2/316.2*, 360.2/245.1 | 130 | 28, 39 | |
flumequine (氟甲喹) | 4.76 | 262.1/244.1*, 262.1/202.1 | 130 | 30, 44 | |
fleroxacin (氟罗沙星) | 3.07 | 370.1/326.1*, 370.1/269.1 | 140 | 27, 38 | |
ciprofloxacin (环丙沙星) | 3.12 | 332.1/314.1*, 332.1/231.1 | 150 | 32, 50 | |
lomefloxacin (洛美沙星) | 3.25 | 352.1/265.1*, 352.1/308.1 | 150 | 33, 25 | |
marbofloxacin (麻保沙星) | 2.94 | 363.1/72.1*, 363.1/345.1 | 125 | 40, 30 | |
nalidixic acid (萘啶酸) | 4.66 | 233.1/187.1*, 233.1/215.1 | 110 | 36, 23 | |
norfloxacin (诺氟沙星) | 3.04 | 320.1/276.2*, 320.1/302.1 | 140 | 25, 33 | |
pefloxacin (培氟沙星) | 3.10 | 334.1/316.1*, 334.1/290.1 | 130 | 33, 26 | |
sarafloxacin (沙拉沙星) | 3.59 | 386.1/342.1*, 386.1/299.1 | 150 | 27, 40 | |
difloxacin (双氟沙星) | 3.64 | 400.1/356.1*, 400.1/299.1 | 140 | 29, 42 | |
sparfloxacin (司帕沙星) | 3.62 | 393.2/349.2*, 393.2/292.1 | 155 | 29, 36 | |
cinoxacin (思诺沙星) | 3.80 | 263.1/217.1*, 263.1/245.1 | 140 | 34, 27 | |
ofloxacin (氧氟沙星) | 3.07 | 362.1/318.1*, 362.1/261.1 | 130 | 27, 39 | |
enoxacin (依诺沙星) | 2.94 | 321.1/303.1*, 321.1/232.1 | 130 | 31, 49 | |
Sulfonamides | sulfapyridine (磺胺吡啶) | 2.39 | 250.1/156.0*, 250.1/184.1 | 90 | 25, 23 |
sulfameter (磺胺对甲氧嘧啶) | 3.20 | 281.1/156.0*, 281.1/126.1 | 80 | 25, 40 | |
sulfamethazine (磺胺二甲嘧啶) | 3.10 | 279.1/186.1*, 279.1/124.1 | 80 | 22, 40 | |
sulfisoxazole (磺胺二甲异噁唑) | 3.98 | 268.1/156.0*, 268.1/113.1 | 110 | 22, 25 | |
sulfisomidine (磺胺二甲异嘧啶) | 3.10 | 279.1/156.0*, 279.1/186.1 | 120 | 28, 26 | |
sulfamethoxazole (磺胺甲噁唑) | 3.82 | 254.1/156.0*, 254.1/108.1 | 80 | 24, 37 | |
sulfamerazine (磺胺甲基嘧啶) | 2.63 | 265.1/156.0*, 265.1/172.0 | 70 | 25, 25 | |
sulfamethizole (磺胺甲噻二唑) | 3.17 | 271.1/156.0*, 271.1/108.0 | 100 | 22, 37 | |
sulfamethoxypyridazine (磺胺甲氧哒嗪) | 3.20 | 281.1/156.0*, 281.1/126.1 | 110 | 26, 35 | |
sulfadimethoxine (磺胺间二甲氧嘧啶) | 4.27 | 311.1/156.1*, 311.1/108.1 | 120 | 30, 40 | |
sulfamonomethoxine (磺胺间甲氧嘧啶) | 3.51 | 281.1/156.1*, 281.1/126.1 | 80 | 22, 39 | |
sulfaquinoxaline (磺胺喹噁啉) | 4.27 | 301.1/156.0*, 301.1/108.0 | 80 | 21, 40 | |
sulfadoxin (磺胺邻二甲氧嘧啶) | 3.78 | 311.1/156.1*, 311.1/108.0 | 100 | 26, 36 | |
sulfachloropyridazine (磺胺氯哒嗪) | 3.62 | 285.1/156.0*, 285.1/108.0 | 110 | 24, 37 | |
sulfadiazine (磺胺嘧啶) | 1.85 | 251.1/156.0*, 251.1/108.1 | 70 | 24, 37 | |
sulfathiazole (磺胺噻唑) | 2.24 | 256.0/156.0*, 256.0/108.1 | 110 | 23, 35 | |
Macrolides | erythromycin (红霉素) | 4.58 | 734.4/158.2*, 734.4/576.4 | 110 | 40, 27 |
tilmicosin (替米考星) | 4.27 | 869.5/174.2*, 869.5/696.5 | 110 | 57, 55 | |
Nitroimidazoles | metronidazole (甲硝唑) | 1.40 | 172.1/128.0*, 172.1/82.0 | 85 | 21, 35 |
metronidazole-OH (羟基甲硝唑) | 1.20 | 188.0/123.1*, 188.0/126.0 | 85 | 20, 23 | |
dimetridazole (地美硝唑) | 1.78 | 142.1/96.0*, 142.1/81.0 | 85 | 22, 36 | |
hydroxydimetridazole (羟甲基甲硝咪唑) | 1.47 | 158.0/140.1*, 158.0/55.0 | 85 | 18, 32 | |
ronidazole (洛硝哒唑) | 1.82 | 201.0/140.1*, 201.0/55.1 | 80 | 18, 32 | |
ipronidazole (异丙硝唑) | 3.90 | 170.1/124.0*, 170.1/109.1 | 90 | 24, 35 | |
ipronidazole-OH (羟基异丙硝唑) | 3.17 | 186.1/168.0*, 186.1/122.0 | 85 | 20, 29 | |
Antiviral | amantadine (金刚烷胺) | 3.08 | 152.2/135.1*, 152.2/93.1 | 90 | 25, 39 |
rimantadine (金刚乙胺) | 4.08 | 180.2/163.2*, 180.2/121.1 | 90 | 23, 34 | |
Chloramphenicols | florfenicol amine (氟苯尼考胺) | 0.91 | 248.2/230.2*, 248.2/130.2 | 75 | 19, 35 |
chloramphenicol (氯霉素) | 4.11 | 321.0/152.0*, 321.0/257.0 | -85 | -25, -16 | |
florfenicol (氟苯尼考) | 3.87 | 356.0/336.0*, 356.0/185.0 | -85 | -14, -27 | |
thiamphenicol (甲砜霉素) | 3.07 | 354.0/185.0*, 354.0/290.0 | -95 | -30, -18 |
表1 50种分析物的保留时间及主要质谱参数
Table 1 Retention times and main MS parameters of the 50 compounds
Type | Compound | tR/min | Qualitative ions (m/z) | Declustering potential/V | Collision energies/eV |
---|---|---|---|---|---|
Fluoroquinolones | orbiflixacin (奥比沙星) | 3.41 | 396.1/352.1*, 396.1/295.1 | 150 | 27, 34 |
pipemidic acid (吡哌酸) | 2.36 | 304.2/217.2*, 304.2/189.1 | 150 | 32, 42 | |
danofloxacin (丹诺沙星) | 3.23 | 358.1/340.1*, 358.1/283.1 | 140 | 35, 34 | |
oxolinic acid (噁喹酸) | 4.06 | 262.1/244.1*, 262.1/216.1 | 130 | 29, 40 | |
enrofloxacin (恩诺沙星) | 3.33 | 360.2/316.2*, 360.2/245.1 | 130 | 28, 39 | |
flumequine (氟甲喹) | 4.76 | 262.1/244.1*, 262.1/202.1 | 130 | 30, 44 | |
fleroxacin (氟罗沙星) | 3.07 | 370.1/326.1*, 370.1/269.1 | 140 | 27, 38 | |
ciprofloxacin (环丙沙星) | 3.12 | 332.1/314.1*, 332.1/231.1 | 150 | 32, 50 | |
lomefloxacin (洛美沙星) | 3.25 | 352.1/265.1*, 352.1/308.1 | 150 | 33, 25 | |
marbofloxacin (麻保沙星) | 2.94 | 363.1/72.1*, 363.1/345.1 | 125 | 40, 30 | |
nalidixic acid (萘啶酸) | 4.66 | 233.1/187.1*, 233.1/215.1 | 110 | 36, 23 | |
norfloxacin (诺氟沙星) | 3.04 | 320.1/276.2*, 320.1/302.1 | 140 | 25, 33 | |
pefloxacin (培氟沙星) | 3.10 | 334.1/316.1*, 334.1/290.1 | 130 | 33, 26 | |
sarafloxacin (沙拉沙星) | 3.59 | 386.1/342.1*, 386.1/299.1 | 150 | 27, 40 | |
difloxacin (双氟沙星) | 3.64 | 400.1/356.1*, 400.1/299.1 | 140 | 29, 42 | |
sparfloxacin (司帕沙星) | 3.62 | 393.2/349.2*, 393.2/292.1 | 155 | 29, 36 | |
cinoxacin (思诺沙星) | 3.80 | 263.1/217.1*, 263.1/245.1 | 140 | 34, 27 | |
ofloxacin (氧氟沙星) | 3.07 | 362.1/318.1*, 362.1/261.1 | 130 | 27, 39 | |
enoxacin (依诺沙星) | 2.94 | 321.1/303.1*, 321.1/232.1 | 130 | 31, 49 | |
Sulfonamides | sulfapyridine (磺胺吡啶) | 2.39 | 250.1/156.0*, 250.1/184.1 | 90 | 25, 23 |
sulfameter (磺胺对甲氧嘧啶) | 3.20 | 281.1/156.0*, 281.1/126.1 | 80 | 25, 40 | |
sulfamethazine (磺胺二甲嘧啶) | 3.10 | 279.1/186.1*, 279.1/124.1 | 80 | 22, 40 | |
sulfisoxazole (磺胺二甲异噁唑) | 3.98 | 268.1/156.0*, 268.1/113.1 | 110 | 22, 25 | |
sulfisomidine (磺胺二甲异嘧啶) | 3.10 | 279.1/156.0*, 279.1/186.1 | 120 | 28, 26 | |
sulfamethoxazole (磺胺甲噁唑) | 3.82 | 254.1/156.0*, 254.1/108.1 | 80 | 24, 37 | |
sulfamerazine (磺胺甲基嘧啶) | 2.63 | 265.1/156.0*, 265.1/172.0 | 70 | 25, 25 | |
sulfamethizole (磺胺甲噻二唑) | 3.17 | 271.1/156.0*, 271.1/108.0 | 100 | 22, 37 | |
sulfamethoxypyridazine (磺胺甲氧哒嗪) | 3.20 | 281.1/156.0*, 281.1/126.1 | 110 | 26, 35 | |
sulfadimethoxine (磺胺间二甲氧嘧啶) | 4.27 | 311.1/156.1*, 311.1/108.1 | 120 | 30, 40 | |
sulfamonomethoxine (磺胺间甲氧嘧啶) | 3.51 | 281.1/156.1*, 281.1/126.1 | 80 | 22, 39 | |
sulfaquinoxaline (磺胺喹噁啉) | 4.27 | 301.1/156.0*, 301.1/108.0 | 80 | 21, 40 | |
sulfadoxin (磺胺邻二甲氧嘧啶) | 3.78 | 311.1/156.1*, 311.1/108.0 | 100 | 26, 36 | |
sulfachloropyridazine (磺胺氯哒嗪) | 3.62 | 285.1/156.0*, 285.1/108.0 | 110 | 24, 37 | |
sulfadiazine (磺胺嘧啶) | 1.85 | 251.1/156.0*, 251.1/108.1 | 70 | 24, 37 | |
sulfathiazole (磺胺噻唑) | 2.24 | 256.0/156.0*, 256.0/108.1 | 110 | 23, 35 | |
Macrolides | erythromycin (红霉素) | 4.58 | 734.4/158.2*, 734.4/576.4 | 110 | 40, 27 |
tilmicosin (替米考星) | 4.27 | 869.5/174.2*, 869.5/696.5 | 110 | 57, 55 | |
Nitroimidazoles | metronidazole (甲硝唑) | 1.40 | 172.1/128.0*, 172.1/82.0 | 85 | 21, 35 |
metronidazole-OH (羟基甲硝唑) | 1.20 | 188.0/123.1*, 188.0/126.0 | 85 | 20, 23 | |
dimetridazole (地美硝唑) | 1.78 | 142.1/96.0*, 142.1/81.0 | 85 | 22, 36 | |
hydroxydimetridazole (羟甲基甲硝咪唑) | 1.47 | 158.0/140.1*, 158.0/55.0 | 85 | 18, 32 | |
ronidazole (洛硝哒唑) | 1.82 | 201.0/140.1*, 201.0/55.1 | 80 | 18, 32 | |
ipronidazole (异丙硝唑) | 3.90 | 170.1/124.0*, 170.1/109.1 | 90 | 24, 35 | |
ipronidazole-OH (羟基异丙硝唑) | 3.17 | 186.1/168.0*, 186.1/122.0 | 85 | 20, 29 | |
Antiviral | amantadine (金刚烷胺) | 3.08 | 152.2/135.1*, 152.2/93.1 | 90 | 25, 39 |
rimantadine (金刚乙胺) | 4.08 | 180.2/163.2*, 180.2/121.1 | 90 | 23, 34 | |
Chloramphenicols | florfenicol amine (氟苯尼考胺) | 0.91 | 248.2/230.2*, 248.2/130.2 | 75 | 19, 35 |
chloramphenicol (氯霉素) | 4.11 | 321.0/152.0*, 321.0/257.0 | -85 | -25, -16 | |
florfenicol (氟苯尼考) | 3.87 | 356.0/336.0*, 356.0/185.0 | -85 | -14, -27 | |
thiamphenicol (甲砜霉素) | 3.07 | 354.0/185.0*, 354.0/290.0 | -95 | -30, -18 |
Compound type | Recoveries under different acidic conditions/% | |||
---|---|---|---|---|
0.1% | 0.5% | 1% | 5% | |
Fluoroquinolones | 62.58-81.36 | 64.67-90.27 | 82.42-113.3 | 82.77-114.8 |
Sulfonamides | 39.14-53.82 | 51.92-70.05 | 65.36-94.07 | 73.77-114.4 |
Macrolides | 55.82-71.64 | 67.67-78.83 | 76.98-96.74 | 80.81-94.75 |
Nitroimidazoles | 63.13-86.54 | 79.24-97.55 | 87.88-112.9 | 95.50-113.7 |
Antiviral | 67.33-89.85 | 84.09-95.55 | 83.70-96.96 | 90.46-101.2 |
Chloramphenicols | 87.73-103.4 | 89.61-110.7 | 98.78-109.0 | 92.37-110.3 |
表2 不同酸性条件下6大类兽药的回收率
Table 2 Recoveries of the six categories of veterinary drugs under different acidic conditions
Compound type | Recoveries under different acidic conditions/% | |||
---|---|---|---|---|
0.1% | 0.5% | 1% | 5% | |
Fluoroquinolones | 62.58-81.36 | 64.67-90.27 | 82.42-113.3 | 82.77-114.8 |
Sulfonamides | 39.14-53.82 | 51.92-70.05 | 65.36-94.07 | 73.77-114.4 |
Macrolides | 55.82-71.64 | 67.67-78.83 | 76.98-96.74 | 80.81-94.75 |
Nitroimidazoles | 63.13-86.54 | 79.24-97.55 | 87.88-112.9 | 95.50-113.7 |
Antiviral | 67.33-89.85 | 84.09-95.55 | 83.70-96.96 | 90.46-101.2 |
Chloramphenicols | 87.73-103.4 | 89.61-110.7 | 98.78-109.0 | 92.37-110.3 |
Compound | Linear equation | r | LOD/(μg/kg) | LOQ/(μg/kg) |
---|---|---|---|---|
Orbiflixacin | Y=197779X+3757 | 0.9996 | 0.22 | 0.75 |
Pipemidic acid | Y=87903X-6529 | 0.9992 | 0.46 | 1.53 |
Danofloxacin | Y=188157X+53899 | 0.9963 | 0.20 | 0.67 |
Oxolinic acid | Y=435877X+192489 | 0.9951 | 0.15 | 0.49 |
Enrofloxacin | Y=132617X-15113 | 0.9990 | 0.18 | 0.58 |
Flumequine | Y=522215X+176642 | 0.9967 | 0.09 | 0.30 |
Fleroxacin | Y=176090X+10428 | 0.9993 | 0.36 | 1.21 |
Ciprofloxacin | Y=107427X+55346 | 0.9954 | 0.46 | 1.54 |
Lomefloxacin | Y=132101X+9999 | 0.9993 | 0.13 | 0.44 |
Marbofloxacin | Y=60345X+3338 | 0.9992 | 0.36 | 1.19 |
Nalidixic acid | Y=298336X+65419 | 0.9980 | 0.16 | 0.53 |
Norfloxacin | Y=51835X-4201 | 0.9991 | 0.30 | 1.02 |
Pefloxacin | Y=237291X+105448 | 0.9957 | 0.19 | 0.65 |
Sarafloxacin | Y=87118X+6292 | 0.9982 | 0.20 | 0.66 |
Difloxacin | Y=128580X-4878 | 0.9987 | 0.30 | 1.00 |
Sparfloxacin | Y=185686X+4122 | 0.9997 | 0.09 | 0.29 |
Cinoxacin | Y=36291X+15880 | 0.9983 | 0.70 | 2.33 |
Ofloxacin | Y=175488X+19008 | 0.9992 | 0.23 | 0.77 |
Enoxacin | Y=285481X-9663 | 0.9982 | 0.13 | 0.44 |
Sulfapyridine | Y=265262X+94227 | 0.9988 | 0.24 | 0.80 |
Sulfameter | Y=428447X+538403 | 0.9960 | 0.23 | 0.77 |
Sulfamethazine | Y=234091X+246581 | 0.9951 | 0.14 | 0.48 |
Sulfisoxazole | Y=218544X+130177 | 0.9962 | 0.16 | 0.54 |
Sulfisomidine | Y=101459X+97429 | 0.9956 | 0.11 | 0.35 |
Sulfamethoxazole | Y=207321X+132074 | 0.9958 | 0.18 | 0.60 |
Sulfamerazine | Y=263730X+72356 | 0.9995 | 0.21 | 0.70 |
Sulfamethizole | Y=184920X+247013 | 0.9956 | 0.34 | 1.14 |
Sulfamethoxypyridazine | Y=384016X+525753 | 0.9954 | 0.03 | 0.11 |
Sulfadimethoxine | Y=525803X+461027 | 0.9970 | 0.07 | 0.24 |
Sulfamonomethoxine | Y=191571X+104637 | 0.9964 | 0.17 | 0.57 |
Sulfaquinoxalin | Y=199160X+310288 | 0.9955 | 0.15 | 0.51 |
Sulfadoxin | Y=538404X+448887 | 0.9958 | 0.21 | 0.70 |
Sulfachloropyridazine | Y=160264X+204651 | 0.9963 | 0.11 | 0.35 |
Sulfadiazine | Y=288292X+127803 | 0.9991 | 0.19 | 0.63 |
Sulfathiazole | Y=274049X+123238 | 0.9955 | 0.13 | 0.42 |
Erythromycin | Y=175371X+61139 | 0.9973 | 0.06 | 0.21 |
Tilmicosin | Y=26547X-8005 | 0.9953 | 0.26 | 0.87 |
Compound | Linear equation | r | LOD/(μg/kg) | LOQ/(μg/kg) |
Metronidazole | Y=360232X+61918 | 0.9976 | 0.03 | 0.09 |
Metronidazole-OH | Y=83637X+11760 | 0.9989 | 0.22 | 0.75 |
Dimetridazole | Y=211275X+13791 | 0.9994 | 0.09 | 0.31 |
Hydroxydimetridazole | Y=141242X+5589 | 0.9986 | 0.26 | 0.87 |
Ronidazole | Y=185802X+65378 | 0.9973 | 0.31 | 1.03 |
Ipronidazole | Y=428540X+40596 | 0.9981 | 0.22 | 0.73 |
Ipronidazole-OH | Y=364488X+19279 | 0.9984 | 0.24 | 0.79 |
Amantadine | Y=902516X+181596 | 0.9981 | 0.52 | 1.73 |
Rimantadine | Y=103634X+256309 | 0.9961 | 0.07 | 0.25 |
Florfenicol amine | Y=140548X+43509 | 0.9954 | 0.09 | 0.31 |
Chloramphenicol | Y=30477X+576 | 0.9990 | 0.36 | 1.21 |
Florfenicol | Y=45215X+8278 | 0.9980 | 0.17 | 0.58 |
Thiamphenicol | Y=10223X+186 | 0.9980 | 0.33 | 1.09 |
表3 50种兽药的线性关系、LOD和LOQ
Table 3 Linear relationships, LODs, and LOQs of the 50 veterinary drugs
Compound | Linear equation | r | LOD/(μg/kg) | LOQ/(μg/kg) |
---|---|---|---|---|
Orbiflixacin | Y=197779X+3757 | 0.9996 | 0.22 | 0.75 |
Pipemidic acid | Y=87903X-6529 | 0.9992 | 0.46 | 1.53 |
Danofloxacin | Y=188157X+53899 | 0.9963 | 0.20 | 0.67 |
Oxolinic acid | Y=435877X+192489 | 0.9951 | 0.15 | 0.49 |
Enrofloxacin | Y=132617X-15113 | 0.9990 | 0.18 | 0.58 |
Flumequine | Y=522215X+176642 | 0.9967 | 0.09 | 0.30 |
Fleroxacin | Y=176090X+10428 | 0.9993 | 0.36 | 1.21 |
Ciprofloxacin | Y=107427X+55346 | 0.9954 | 0.46 | 1.54 |
Lomefloxacin | Y=132101X+9999 | 0.9993 | 0.13 | 0.44 |
Marbofloxacin | Y=60345X+3338 | 0.9992 | 0.36 | 1.19 |
Nalidixic acid | Y=298336X+65419 | 0.9980 | 0.16 | 0.53 |
Norfloxacin | Y=51835X-4201 | 0.9991 | 0.30 | 1.02 |
Pefloxacin | Y=237291X+105448 | 0.9957 | 0.19 | 0.65 |
Sarafloxacin | Y=87118X+6292 | 0.9982 | 0.20 | 0.66 |
Difloxacin | Y=128580X-4878 | 0.9987 | 0.30 | 1.00 |
Sparfloxacin | Y=185686X+4122 | 0.9997 | 0.09 | 0.29 |
Cinoxacin | Y=36291X+15880 | 0.9983 | 0.70 | 2.33 |
Ofloxacin | Y=175488X+19008 | 0.9992 | 0.23 | 0.77 |
Enoxacin | Y=285481X-9663 | 0.9982 | 0.13 | 0.44 |
Sulfapyridine | Y=265262X+94227 | 0.9988 | 0.24 | 0.80 |
Sulfameter | Y=428447X+538403 | 0.9960 | 0.23 | 0.77 |
Sulfamethazine | Y=234091X+246581 | 0.9951 | 0.14 | 0.48 |
Sulfisoxazole | Y=218544X+130177 | 0.9962 | 0.16 | 0.54 |
Sulfisomidine | Y=101459X+97429 | 0.9956 | 0.11 | 0.35 |
Sulfamethoxazole | Y=207321X+132074 | 0.9958 | 0.18 | 0.60 |
Sulfamerazine | Y=263730X+72356 | 0.9995 | 0.21 | 0.70 |
Sulfamethizole | Y=184920X+247013 | 0.9956 | 0.34 | 1.14 |
Sulfamethoxypyridazine | Y=384016X+525753 | 0.9954 | 0.03 | 0.11 |
Sulfadimethoxine | Y=525803X+461027 | 0.9970 | 0.07 | 0.24 |
Sulfamonomethoxine | Y=191571X+104637 | 0.9964 | 0.17 | 0.57 |
Sulfaquinoxalin | Y=199160X+310288 | 0.9955 | 0.15 | 0.51 |
Sulfadoxin | Y=538404X+448887 | 0.9958 | 0.21 | 0.70 |
Sulfachloropyridazine | Y=160264X+204651 | 0.9963 | 0.11 | 0.35 |
Sulfadiazine | Y=288292X+127803 | 0.9991 | 0.19 | 0.63 |
Sulfathiazole | Y=274049X+123238 | 0.9955 | 0.13 | 0.42 |
Erythromycin | Y=175371X+61139 | 0.9973 | 0.06 | 0.21 |
Tilmicosin | Y=26547X-8005 | 0.9953 | 0.26 | 0.87 |
Compound | Linear equation | r | LOD/(μg/kg) | LOQ/(μg/kg) |
Metronidazole | Y=360232X+61918 | 0.9976 | 0.03 | 0.09 |
Metronidazole-OH | Y=83637X+11760 | 0.9989 | 0.22 | 0.75 |
Dimetridazole | Y=211275X+13791 | 0.9994 | 0.09 | 0.31 |
Hydroxydimetridazole | Y=141242X+5589 | 0.9986 | 0.26 | 0.87 |
Ronidazole | Y=185802X+65378 | 0.9973 | 0.31 | 1.03 |
Ipronidazole | Y=428540X+40596 | 0.9981 | 0.22 | 0.73 |
Ipronidazole-OH | Y=364488X+19279 | 0.9984 | 0.24 | 0.79 |
Amantadine | Y=902516X+181596 | 0.9981 | 0.52 | 1.73 |
Rimantadine | Y=103634X+256309 | 0.9961 | 0.07 | 0.25 |
Florfenicol amine | Y=140548X+43509 | 0.9954 | 0.09 | 0.31 |
Chloramphenicol | Y=30477X+576 | 0.9990 | 0.36 | 1.21 |
Florfenicol | Y=45215X+8278 | 0.9980 | 0.17 | 0.58 |
Thiamphenicol | Y=10223X+186 | 0.9980 | 0.33 | 1.09 |
Compound | Spiked/ (μg/kg) | Mean recoveries/% | RSDs/% | |||||
---|---|---|---|---|---|---|---|---|
Rice powder | Meat paste | Fish paste | Rice powder | Meat paste | Fish paste | |||
Orbiflixacin | 5 | 87.09 | 111.7 | 95.45 | 9.2 | 5.1 | 6.7 | |
50 | 90.40 | 90.36 | 92.02 | 5.9 | 5.6 | 7.8 | ||
Pipemidic acid | 5 | 114.1 | 100.5 | 91.28 | 7.7 | 9.4 | 3.5 | |
50 | 94.10 | 83.39 | 88.21 | 8.7 | 6.4 | 7.4 | ||
Danofloxacin | 5 | 83.69 | 90.52 | 75.61 | 9.4 | 4.9 | 6.8 | |
50 | 75.51 | 86.03 | 81.89 | 5.9 | 7.2 | 7.0 | ||
Oxolinic acid | 5 | 102.7 | 84.29 | 83.47 | 9.4 | 6.3 | 8.5 | |
50 | 85.82 | 71.83 | 73.68 | 9.1 | 6.3 | 7.0 | ||
Enrofloxacin | 5 | 106.4 | 111.8 | 87.26 | 8.4 | 5.5 | 7.4 | |
50 | 75.73 | 89.95 | 95.11 | 6.6 | 5.3 | 6.7 | ||
Compound | Spiked/ (μg/kg) | Mean recoveries/% | RSDs/% | |||||
Rice powder | Meat paste | Fish paste | Rice powder | Meat paste | Fish paste | |||
Sulfadoxin | 5 | 84.01 | 116.8 | 111.3 | 7.4 | 10.3 | 9.9 | |
50 | 92.79 | 95.47 | 107.1 | 13.0 | 8.4 | 7.6 | ||
Sulfachloropyridazine | 5 | 73.95 | 117.8 | 113.8 | 11.5 | 10.5 | 10.0 | |
50 | 95.65 | 71.25 | 110.7 | 6.1 | 9.1 | 9.2 | ||
Sulfadiazine | 5 | 95.94 | 74.07 | 108.7 | 8.2 | 15.4 | 12.7 | |
50 | 81.12 | 99.27 | 101.8 | 11.2 | 9.0 | 10.2 | ||
Sulfathiazole | 5 | 101.4 | 72.91 | 112.7 | 5.7 | 11.7 | 10.8 | |
50 | 88.96 | 106.7 | 115.6 | 11.7 | 9.4 | 10.0 | ||
Erythromycin | 5 | 73.91 | 75.24 | 70.94 | 7.5 | 7.2 | 7.5 | |
50 | 76.99 | 79.09 | 93.23 | 5.0 | 6.2 | 6.8 | ||
Tilmicosin | 5 | 81.95 | 69.36 | 65.62 | 10.0 | 7.9 | 8.1 | |
50 | 101.3 | 74.52 | 105.1 | 3.9 | 6.0 | 6.2 | ||
Metronidazole | 5 | 71.70 | 101.2 | 87.15 | 9.7 | 8.7 | 8.3 | |
50 | 103.3 | 97.19 | 92.18 | 11.6 | 10.1 | 10.0 | ||
Metronidazole-OH | 5 | 100.9 | 93.29 | 97.64 | 12.1 | 6.2 | 7.3 | |
50 | 112.8 | 91.75 | 90.04 | 1.1 | 6.7 | 7.0 | ||
Dimetridazole | 5 | 93.93 | 100.1 | 86.08 | 4.0 | 8.3 | 8.0 | |
50 | 78.25 | 93.13 | 88.35 | 10.8 | 5.2 | 5.9 | ||
Hydroxydimetridazole | 5 | 88.88 | 104.7 | 94.76 | 12.1 | 6.6 | 6.5 | |
50 | 100.1 | 78.73 | 89.15 | 9.5 | 8.7 | 8.7 | ||
Ronidazole | 5 | 78.79 | 84.58 | 86.26 | 9.0 | 7.2 | 6.9 | |
50 | 104.8 | 81.04 | 78.18 | 9.2 | 8.8 | 8.4 | ||
Ipronidazole | 5 | 97.68 | 104.4 | 87.36 | 6.3 | 9.5 | 8.8 | |
50 | 76.53 | 73.83 | 83.44 | 8.4 | 7.0 | 5.0 | ||
Ipronidazole-OH | 5 | 98.43 | 93.35 | 94.63 | 11.5 | 13.2 | 10.5 | |
50 | 89.16 | 88.68 | 97.34 | 1.6 | 9.9 | 11.9 | ||
Amantadine | 5 | 96.22 | 106.5 | 90.41 | 13.1 | 9.1 | 8.6 | |
50 | 72.36 | 115.3 | 83.61 | 5.6 | 9.2 | 12.7 | ||
Rimantadine | 5 | 92.25 | 110.8 | 85.47 | 8.7 | 9.7 | 10.8 | |
50 | 80.56 | 92.11 | 93.45 | 12.5 | 8.9 | 9.9 | ||
Florfenicol amine | 5 | 108.7 | 85.03 | 93.02 | 12.7 | 10.3 | 9.5 | |
50 | 109.6 | 66.41 | 66.53 | 13.6 | 9.7 | 11.9 | ||
Chloramphenicol | 5 | 112.1 | 82.14 | 103.1 | 4.4 | 8.9 | 7.7 | |
50 | 95.89 | 91.09 | 88.53 | 3.8 | 5.0 | 7.6 | ||
Florfenicol | 5 | 94.01 | 93.55 | 88.88 | 4.9 | 9.5 | 9.6 | |
50 | 79.85 | 69.99 | 76.68 | 4.3 | 4.3 | 6.9 | ||
Thiamphenicol | 5 | 112.3 | 104.2 | 86.17 | 9.0 | 11.8 | 11.5 | |
50 | 89.43 | 92.46 | 83.77 | 8.1 | 7.9 | 6.2 | ||
Compound | Spiked/ (μg/kg) | Mean recoveries/% | RSDs/% | |||||
Rice powder | Meat paste | Fish paste | Rice powder | Meat paste | Fish paste | |||
Flumequine | 5 | 100.4 | 104.1 | 92.64 | 9.1 | 7.1 | 7.5 | |
50 | 94.42 | 75.04 | 88.41 | 6.8 | 6.4 | 6.7 | ||
Fleroxacin | 5 | 100.9 | 104.2 | 86.79 | 7.4 | 8.7 | 6.0 | |
50 | 74.37 | 77.57 | 87.49 | 3.0 | 5.0 | 6.7 | ||
Ciprofloxacin | 5 | 89.67 | 96.55 | 72.07 | 8.5 | 4.8 | 5.8 | |
50 | 77.78 | 64.46 | 82.74 | 6.1 | 3.4 | 5.3 | ||
Lomefloxacin | 5 | 76.96 | 106.4 | 93.43 | 8.2 | 9.1 | 6.7 | |
50 | 89.95 | 82.33 | 100.4 | 7.2 | 5.9 | 6.9 | ||
Marbofloxacin | 5 | 100.7 | 97.42 | 83.69 | 5.7 | 6.8 | 7.9 | |
50 | 78.06 | 89.07 | 74.11 | 8.7 | 3.2 | 3.9 | ||
Nalidixic acid | 5 | 110.8 | 101.9 | 104.7 | 7.5 | 12.8 | 13.2 | |
50 | 91.44 | 75.97 | 85.73 | 5.0 | 2.9 | 3.1 | ||
Norfloxacin | 5 | 107.1 | 117.0 | 87.09 | 9.9 | 12.7 | 11.2 | |
50 | 73.39 | 68.92 | 90.16 | 3.9 | 3.8 | 3.8 | ||
Pefloxacin | 5 | 81.53 | 88.48 | 78.17 | 9.7 | 2.7 | 3.3 | |
50 | 79.95 | 77.69 | 79.05 | 5.6 | 3.1 | 4.2 | ||
Sarafloxacin | 5 | 87.51 | 96.72 | 89.64 | 2.1 | 2.7 | 3.6 | |
50 | 80.33 | 74.90 | 80.27 | 1.1 | 3.0 | 3.5 | ||
Difloxacin | 5 | 110.4 | 92.96 | 89.36 | 4.0 | 2.8 | 2.8 | |
50 | 104.0 | 68.44 | 73.34 | 9.8 | 2.2 | 2.5 | ||
Sparfloxacin | 5 | 84.06 | 109.2 | 85.54 | 8.1 | 2.3 | 2.0 | |
50 | 106.2 | 96.94 | 102.5 | 9.5 | 2.7 | 3.1 | ||
Cinoxacin | 5 | 104.8 | 80.66 | 107.9 | 9.0 | 1.4 | 1.5 | |
50 | 114.8 | 94.21 | 83.74 | 9.2 | 2.7 | 3.0 | ||
Ofloxacin | 5 | 96.53 | 97.44 | 77.18 | 6.3 | 2.2 | 3.4 | |
50 | 78.29 | 94.11 | 89.93 | 8.4 | 3.7 | 5.4 | ||
Enoxacin | 5 | 109.3 | 83.36 | 91.15 | 4.5 | 7.7 | 6.4 | |
50 | 79.56 | 64.57 | 64.37 | 6.6 | 4.2 | 5.9 | ||
Sulfapyridine | 5 | 93.52 | 81.84 | 104.2 | 13.1 | 9.8 | 13.8 | |
50 | 70.60 | 100.4 | 104.9 | 5.6 | 6.5 | 6.8 | ||
Sulfameter | 5 | 79.39 | 82.05 | 100.5 | 8.7 | 6.6 | 8.8 | |
50 | 86.36 | 108.1 | 115.2 | 5.5 | 5.9 | 6.6 | ||
Sulfamethazine | 5 | 75.18 | 86.67 | 93.64 | 6.7 | 6.7 | 8.2 | |
50 | 72.79 | 113.6 | 119.3 | 8.6 | 6.4 | 9.0 | ||
Sulfisoxazole | 5 | 106.0 | 68.55 | 114.4 | 3.8 | 5.8 | 8.1 | |
50 | 83.93 | 86.66 | 110.6 | 4.9 | 4.2 | 7.0 | ||
Sulfisomidine | 5 | 91.08 | 114.3 | 98.13 | 4.4 | 5.3 | 5.9 | |
50 | 76.24 | 95.98 | 112.1 | 9.3 | 8.6 | 7.4 | ||
Sulfamethoxazole | 5 | 114.7 | 69.31 | 110.3 | 9.0 | 7.9 | 4.6 | |
50 | 92.69 | 69.54 | 107.2 | 8.1 | 8.0 | 5.5 | ||
Sulfamerazine | 5 | 106.6 | 71.07 | 106.1 | 13.2 | 8.3 | 7.1 | |
50 | 74.54 | 112.1 | 98.37 | 5.9 | 11.0 | 11.4 | ||
Sulfamethizole | 5 | 95.27 | 98.16 | 109.6 | 7.7 | 14.4 | 12.5 | |
50 | 98.85 | 78.12 | 118.8 | 10.0 | 9.8 | 9.8 | ||
Sulfamethoxypyridazine | 5 | 74.90 | 83.97 | 97.16 | 9.4 | 9.7 | 8.7 | |
50 | 86.92 | 96.46 | 105.3 | 5.9 | 8.8 | 11.2 | ||
Sulfadimethoxine | 5 | 84.69 | 71.66 | 107.6 | 9.4 | 10.6 | 9.5 | |
50 | 83.72 | 68.66 | 79.74 | 9.1 | 9.9 | 10.6 | ||
Sulfamonomethoxine | 5 | 87.14 | 114.8 | 100.5 | 8.4 | 8.4 | 9.1 | |
50 | 94.13 | 113.2 | 117.3 | 10.6 | 11.4 | 11.6 | ||
Sulfaquinoxalin | 5 | 89.66 | 115.8 | 106.4 | 9.1 | 13.5 | 12.4 | |
50 | 92.98 | 68.87 | 83.51 | 13.8 | 8.7 | 8.1 |
表4 50种兽药在3种基质中的平均回收率及相对标准偏差(n=6)
Table 4 Mean recoveries and RSDs of the 50 veterinary drugs in three matrices (n=6)
Compound | Spiked/ (μg/kg) | Mean recoveries/% | RSDs/% | |||||
---|---|---|---|---|---|---|---|---|
Rice powder | Meat paste | Fish paste | Rice powder | Meat paste | Fish paste | |||
Orbiflixacin | 5 | 87.09 | 111.7 | 95.45 | 9.2 | 5.1 | 6.7 | |
50 | 90.40 | 90.36 | 92.02 | 5.9 | 5.6 | 7.8 | ||
Pipemidic acid | 5 | 114.1 | 100.5 | 91.28 | 7.7 | 9.4 | 3.5 | |
50 | 94.10 | 83.39 | 88.21 | 8.7 | 6.4 | 7.4 | ||
Danofloxacin | 5 | 83.69 | 90.52 | 75.61 | 9.4 | 4.9 | 6.8 | |
50 | 75.51 | 86.03 | 81.89 | 5.9 | 7.2 | 7.0 | ||
Oxolinic acid | 5 | 102.7 | 84.29 | 83.47 | 9.4 | 6.3 | 8.5 | |
50 | 85.82 | 71.83 | 73.68 | 9.1 | 6.3 | 7.0 | ||
Enrofloxacin | 5 | 106.4 | 111.8 | 87.26 | 8.4 | 5.5 | 7.4 | |
50 | 75.73 | 89.95 | 95.11 | 6.6 | 5.3 | 6.7 | ||
Compound | Spiked/ (μg/kg) | Mean recoveries/% | RSDs/% | |||||
Rice powder | Meat paste | Fish paste | Rice powder | Meat paste | Fish paste | |||
Sulfadoxin | 5 | 84.01 | 116.8 | 111.3 | 7.4 | 10.3 | 9.9 | |
50 | 92.79 | 95.47 | 107.1 | 13.0 | 8.4 | 7.6 | ||
Sulfachloropyridazine | 5 | 73.95 | 117.8 | 113.8 | 11.5 | 10.5 | 10.0 | |
50 | 95.65 | 71.25 | 110.7 | 6.1 | 9.1 | 9.2 | ||
Sulfadiazine | 5 | 95.94 | 74.07 | 108.7 | 8.2 | 15.4 | 12.7 | |
50 | 81.12 | 99.27 | 101.8 | 11.2 | 9.0 | 10.2 | ||
Sulfathiazole | 5 | 101.4 | 72.91 | 112.7 | 5.7 | 11.7 | 10.8 | |
50 | 88.96 | 106.7 | 115.6 | 11.7 | 9.4 | 10.0 | ||
Erythromycin | 5 | 73.91 | 75.24 | 70.94 | 7.5 | 7.2 | 7.5 | |
50 | 76.99 | 79.09 | 93.23 | 5.0 | 6.2 | 6.8 | ||
Tilmicosin | 5 | 81.95 | 69.36 | 65.62 | 10.0 | 7.9 | 8.1 | |
50 | 101.3 | 74.52 | 105.1 | 3.9 | 6.0 | 6.2 | ||
Metronidazole | 5 | 71.70 | 101.2 | 87.15 | 9.7 | 8.7 | 8.3 | |
50 | 103.3 | 97.19 | 92.18 | 11.6 | 10.1 | 10.0 | ||
Metronidazole-OH | 5 | 100.9 | 93.29 | 97.64 | 12.1 | 6.2 | 7.3 | |
50 | 112.8 | 91.75 | 90.04 | 1.1 | 6.7 | 7.0 | ||
Dimetridazole | 5 | 93.93 | 100.1 | 86.08 | 4.0 | 8.3 | 8.0 | |
50 | 78.25 | 93.13 | 88.35 | 10.8 | 5.2 | 5.9 | ||
Hydroxydimetridazole | 5 | 88.88 | 104.7 | 94.76 | 12.1 | 6.6 | 6.5 | |
50 | 100.1 | 78.73 | 89.15 | 9.5 | 8.7 | 8.7 | ||
Ronidazole | 5 | 78.79 | 84.58 | 86.26 | 9.0 | 7.2 | 6.9 | |
50 | 104.8 | 81.04 | 78.18 | 9.2 | 8.8 | 8.4 | ||
Ipronidazole | 5 | 97.68 | 104.4 | 87.36 | 6.3 | 9.5 | 8.8 | |
50 | 76.53 | 73.83 | 83.44 | 8.4 | 7.0 | 5.0 | ||
Ipronidazole-OH | 5 | 98.43 | 93.35 | 94.63 | 11.5 | 13.2 | 10.5 | |
50 | 89.16 | 88.68 | 97.34 | 1.6 | 9.9 | 11.9 | ||
Amantadine | 5 | 96.22 | 106.5 | 90.41 | 13.1 | 9.1 | 8.6 | |
50 | 72.36 | 115.3 | 83.61 | 5.6 | 9.2 | 12.7 | ||
Rimantadine | 5 | 92.25 | 110.8 | 85.47 | 8.7 | 9.7 | 10.8 | |
50 | 80.56 | 92.11 | 93.45 | 12.5 | 8.9 | 9.9 | ||
Florfenicol amine | 5 | 108.7 | 85.03 | 93.02 | 12.7 | 10.3 | 9.5 | |
50 | 109.6 | 66.41 | 66.53 | 13.6 | 9.7 | 11.9 | ||
Chloramphenicol | 5 | 112.1 | 82.14 | 103.1 | 4.4 | 8.9 | 7.7 | |
50 | 95.89 | 91.09 | 88.53 | 3.8 | 5.0 | 7.6 | ||
Florfenicol | 5 | 94.01 | 93.55 | 88.88 | 4.9 | 9.5 | 9.6 | |
50 | 79.85 | 69.99 | 76.68 | 4.3 | 4.3 | 6.9 | ||
Thiamphenicol | 5 | 112.3 | 104.2 | 86.17 | 9.0 | 11.8 | 11.5 | |
50 | 89.43 | 92.46 | 83.77 | 8.1 | 7.9 | 6.2 | ||
Compound | Spiked/ (μg/kg) | Mean recoveries/% | RSDs/% | |||||
Rice powder | Meat paste | Fish paste | Rice powder | Meat paste | Fish paste | |||
Flumequine | 5 | 100.4 | 104.1 | 92.64 | 9.1 | 7.1 | 7.5 | |
50 | 94.42 | 75.04 | 88.41 | 6.8 | 6.4 | 6.7 | ||
Fleroxacin | 5 | 100.9 | 104.2 | 86.79 | 7.4 | 8.7 | 6.0 | |
50 | 74.37 | 77.57 | 87.49 | 3.0 | 5.0 | 6.7 | ||
Ciprofloxacin | 5 | 89.67 | 96.55 | 72.07 | 8.5 | 4.8 | 5.8 | |
50 | 77.78 | 64.46 | 82.74 | 6.1 | 3.4 | 5.3 | ||
Lomefloxacin | 5 | 76.96 | 106.4 | 93.43 | 8.2 | 9.1 | 6.7 | |
50 | 89.95 | 82.33 | 100.4 | 7.2 | 5.9 | 6.9 | ||
Marbofloxacin | 5 | 100.7 | 97.42 | 83.69 | 5.7 | 6.8 | 7.9 | |
50 | 78.06 | 89.07 | 74.11 | 8.7 | 3.2 | 3.9 | ||
Nalidixic acid | 5 | 110.8 | 101.9 | 104.7 | 7.5 | 12.8 | 13.2 | |
50 | 91.44 | 75.97 | 85.73 | 5.0 | 2.9 | 3.1 | ||
Norfloxacin | 5 | 107.1 | 117.0 | 87.09 | 9.9 | 12.7 | 11.2 | |
50 | 73.39 | 68.92 | 90.16 | 3.9 | 3.8 | 3.8 | ||
Pefloxacin | 5 | 81.53 | 88.48 | 78.17 | 9.7 | 2.7 | 3.3 | |
50 | 79.95 | 77.69 | 79.05 | 5.6 | 3.1 | 4.2 | ||
Sarafloxacin | 5 | 87.51 | 96.72 | 89.64 | 2.1 | 2.7 | 3.6 | |
50 | 80.33 | 74.90 | 80.27 | 1.1 | 3.0 | 3.5 | ||
Difloxacin | 5 | 110.4 | 92.96 | 89.36 | 4.0 | 2.8 | 2.8 | |
50 | 104.0 | 68.44 | 73.34 | 9.8 | 2.2 | 2.5 | ||
Sparfloxacin | 5 | 84.06 | 109.2 | 85.54 | 8.1 | 2.3 | 2.0 | |
50 | 106.2 | 96.94 | 102.5 | 9.5 | 2.7 | 3.1 | ||
Cinoxacin | 5 | 104.8 | 80.66 | 107.9 | 9.0 | 1.4 | 1.5 | |
50 | 114.8 | 94.21 | 83.74 | 9.2 | 2.7 | 3.0 | ||
Ofloxacin | 5 | 96.53 | 97.44 | 77.18 | 6.3 | 2.2 | 3.4 | |
50 | 78.29 | 94.11 | 89.93 | 8.4 | 3.7 | 5.4 | ||
Enoxacin | 5 | 109.3 | 83.36 | 91.15 | 4.5 | 7.7 | 6.4 | |
50 | 79.56 | 64.57 | 64.37 | 6.6 | 4.2 | 5.9 | ||
Sulfapyridine | 5 | 93.52 | 81.84 | 104.2 | 13.1 | 9.8 | 13.8 | |
50 | 70.60 | 100.4 | 104.9 | 5.6 | 6.5 | 6.8 | ||
Sulfameter | 5 | 79.39 | 82.05 | 100.5 | 8.7 | 6.6 | 8.8 | |
50 | 86.36 | 108.1 | 115.2 | 5.5 | 5.9 | 6.6 | ||
Sulfamethazine | 5 | 75.18 | 86.67 | 93.64 | 6.7 | 6.7 | 8.2 | |
50 | 72.79 | 113.6 | 119.3 | 8.6 | 6.4 | 9.0 | ||
Sulfisoxazole | 5 | 106.0 | 68.55 | 114.4 | 3.8 | 5.8 | 8.1 | |
50 | 83.93 | 86.66 | 110.6 | 4.9 | 4.2 | 7.0 | ||
Sulfisomidine | 5 | 91.08 | 114.3 | 98.13 | 4.4 | 5.3 | 5.9 | |
50 | 76.24 | 95.98 | 112.1 | 9.3 | 8.6 | 7.4 | ||
Sulfamethoxazole | 5 | 114.7 | 69.31 | 110.3 | 9.0 | 7.9 | 4.6 | |
50 | 92.69 | 69.54 | 107.2 | 8.1 | 8.0 | 5.5 | ||
Sulfamerazine | 5 | 106.6 | 71.07 | 106.1 | 13.2 | 8.3 | 7.1 | |
50 | 74.54 | 112.1 | 98.37 | 5.9 | 11.0 | 11.4 | ||
Sulfamethizole | 5 | 95.27 | 98.16 | 109.6 | 7.7 | 14.4 | 12.5 | |
50 | 98.85 | 78.12 | 118.8 | 10.0 | 9.8 | 9.8 | ||
Sulfamethoxypyridazine | 5 | 74.90 | 83.97 | 97.16 | 9.4 | 9.7 | 8.7 | |
50 | 86.92 | 96.46 | 105.3 | 5.9 | 8.8 | 11.2 | ||
Sulfadimethoxine | 5 | 84.69 | 71.66 | 107.6 | 9.4 | 10.6 | 9.5 | |
50 | 83.72 | 68.66 | 79.74 | 9.1 | 9.9 | 10.6 | ||
Sulfamonomethoxine | 5 | 87.14 | 114.8 | 100.5 | 8.4 | 8.4 | 9.1 | |
50 | 94.13 | 113.2 | 117.3 | 10.6 | 11.4 | 11.6 | ||
Sulfaquinoxalin | 5 | 89.66 | 115.8 | 106.4 | 9.1 | 13.5 | 12.4 | |
50 | 92.98 | 68.87 | 83.51 | 13.8 | 8.7 | 8.1 |
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