Acta Agriculturae Zhejiangensis ›› 2026, Vol. 38 ›› Issue (4): 781-787.DOI: 10.3969/j.issn.1004-1524.20250673
• Quality and Safety of Agricultural Products • Previous Articles Next Articles
QIAN Lingling1(
), QIAN Mingrong2, LIN Hui3, LI Rui1, ZHANG Hu1, YU Ziqing1, WANG Jianmei1,*(
)
Received:2025-11-03
Online:2026-04-25
Published:2026-05-08
Contact:
WANG Jianmei
CLC Number:
QIAN Lingling, QIAN Mingrong, LIN Hui, LI Rui, ZHANG Hu, YU Ziqing, WANG Jianmei. Study on the residue elimination pattern of enrofloxacin and its metabolites in Jiangshan black-bone chickens[J]. Acta Agriculturae Zhejiangensis, 2026, 38(4): 781-787.
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URL: http://www.zjnyxb.cn/EN/10.3969/j.issn.1004-1524.20250673
| t/min | 流速/(mL·min-1) Flow rate/(mL·min-1) | A/% | B/% |
|---|---|---|---|
| 0 | 0.40 | 5 | 95 |
| 2.0 | 0.40 | 20 | 80 |
| 6.5 | 0.40 | 99 | 1 |
| 8.0 | 0.40 | 99 | 1 |
| 8.1 | 0.40 | 5 | 95 |
| 10.0 | 0.40 | 5 | 95 |
Table 1 Gradient elution program
| t/min | 流速/(mL·min-1) Flow rate/(mL·min-1) | A/% | B/% |
|---|---|---|---|
| 0 | 0.40 | 5 | 95 |
| 2.0 | 0.40 | 20 | 80 |
| 6.5 | 0.40 | 99 | 1 |
| 8.0 | 0.40 | 99 | 1 |
| 8.1 | 0.40 | 5 | 95 |
| 10.0 | 0.40 | 5 | 95 |
| 药物 Drug | 定性离子对(m/z) Qualitative ion pairs(m/z) | 定量离子对(m/z) Quantitative ion pairs(m/z) | 去簇电压/V Declustering potential/V | 碰撞能量/eV Collision energy/eV |
|---|---|---|---|---|
| 恩诺沙星 | 360.1>316.0 | 360.1>316.0 | 80 | 23 |
| Enrofloxacin | 360.1>245.4 | 40 | ||
| 环丙沙星 | 332.0>314.0 | 332.0>314.0 | 80 | 25 |
| Ciprofloxacin | 332.0>231.0 | 45 |
Table 2 Ion pairs, declustering potential, and collision energy parameters
| 药物 Drug | 定性离子对(m/z) Qualitative ion pairs(m/z) | 定量离子对(m/z) Quantitative ion pairs(m/z) | 去簇电压/V Declustering potential/V | 碰撞能量/eV Collision energy/eV |
|---|---|---|---|---|
| 恩诺沙星 | 360.1>316.0 | 360.1>316.0 | 80 | 23 |
| Enrofloxacin | 360.1>245.4 | 40 | ||
| 环丙沙星 | 332.0>314.0 | 332.0>314.0 | 80 | 25 |
| Ciprofloxacin | 332.0>231.0 | 45 |
| 组织 Tissue | 恩诺沙星Enrofloxacin | 环丙沙星Ciprofloxacin | ||||||
|---|---|---|---|---|---|---|---|---|
| 标准曲线方程 Calibration curve equation | 相关系数 Correlation coefficient | 回收率/% Recovery/ % | 相对偏差/% Relative deviation/% | 标准曲线方程 Calibration curve equation | 相关系数 Correlation coefficient | 回收率/% Recovery/ % | 相对偏差/% Relative deviation/% | |
| 肌肉Muscle | y=257 920x+207 389 | 0.999 8 | 78.9 | 9.2 | y=481 424x+643 445 | 0.999 1 | 74.4 | 3.8 |
| 肝Liver | y=147 931x+42 976 | 0.999 9 | 68.6 | 11.3 | y=269 635x+59 372 | 0.999 0 | 78.3 | 9.3 |
| 肾Kidney | y=182 878x+92 254 | 1.000 0 | 74.5 | 3.2 | y=344 484x+55 745 | 0.999 9 | 72.2 | 4.3 |
| 皮脂Sebum | y=150 087x+84 190 | 0.999 9 | 73.0 | 4.8 | y=263 916x+11 177 | 0.998 9 | 71.7 | 2.1 |
Table 3 Linearity, recovery and relative deviation of enrofloxacin and ciprofloxacin in different tissues of hens
| 组织 Tissue | 恩诺沙星Enrofloxacin | 环丙沙星Ciprofloxacin | ||||||
|---|---|---|---|---|---|---|---|---|
| 标准曲线方程 Calibration curve equation | 相关系数 Correlation coefficient | 回收率/% Recovery/ % | 相对偏差/% Relative deviation/% | 标准曲线方程 Calibration curve equation | 相关系数 Correlation coefficient | 回收率/% Recovery/ % | 相对偏差/% Relative deviation/% | |
| 肌肉Muscle | y=257 920x+207 389 | 0.999 8 | 78.9 | 9.2 | y=481 424x+643 445 | 0.999 1 | 74.4 | 3.8 |
| 肝Liver | y=147 931x+42 976 | 0.999 9 | 68.6 | 11.3 | y=269 635x+59 372 | 0.999 0 | 78.3 | 9.3 |
| 肾Kidney | y=182 878x+92 254 | 1.000 0 | 74.5 | 3.2 | y=344 484x+55 745 | 0.999 9 | 72.2 | 4.3 |
| 皮脂Sebum | y=150 087x+84 190 | 0.999 9 | 73.0 | 4.8 | y=263 916x+11 177 | 0.998 9 | 71.7 | 2.1 |
| 组织 Tissue | 恩诺沙星Enrofloxacin | 环丙沙星Ciprofloxacin | ||||||
|---|---|---|---|---|---|---|---|---|
| 标准曲线方程 Calibration curve equation | 相关系数 Correlation coefficient | 回收率/% Recovery/ % | 相对偏差/% Relative deviation/% | 标准曲线方程 Calibration curve equation | 相关系数 Correlation coefficient | 回收率/% Recovery/ % | 相对偏差/% Relative deviation/% | |
| 肌肉Muscle | y=223 539x+92 834 | 0.996 2 | 84.4 | 0.8 | y=493 511x+92 496 | 0.998 3 | 82.6 | 8.3 |
| 肝Liver | y=126 668x+99 024 | 0.999 7 | 74.8 | 8.7 | y=222 367x+65 713 | 0.993 4 | 66.8 | 6.7 |
| 肾Kidney | y=177 291x+96 462 | 0.999 0 | 78.1 | 3.5 | y=314 574x+70 553 | 0.997 4 | 66.9 | 3.8 |
| 皮脂Sebum | y=177 370x+91 073 | 0.999 6 | 75.7 | 13.9 | y=285 097x+223 774 | 0.999 3 | 73.2 | 11.7 |
Table 4 Linearity, recovery and relative deviation of enrofloxacin and ciprofloxacin in different tissues of roosters
| 组织 Tissue | 恩诺沙星Enrofloxacin | 环丙沙星Ciprofloxacin | ||||||
|---|---|---|---|---|---|---|---|---|
| 标准曲线方程 Calibration curve equation | 相关系数 Correlation coefficient | 回收率/% Recovery/ % | 相对偏差/% Relative deviation/% | 标准曲线方程 Calibration curve equation | 相关系数 Correlation coefficient | 回收率/% Recovery/ % | 相对偏差/% Relative deviation/% | |
| 肌肉Muscle | y=223 539x+92 834 | 0.996 2 | 84.4 | 0.8 | y=493 511x+92 496 | 0.998 3 | 82.6 | 8.3 |
| 肝Liver | y=126 668x+99 024 | 0.999 7 | 74.8 | 8.7 | y=222 367x+65 713 | 0.993 4 | 66.8 | 6.7 |
| 肾Kidney | y=177 291x+96 462 | 0.999 0 | 78.1 | 3.5 | y=314 574x+70 553 | 0.997 4 | 66.9 | 3.8 |
| 皮脂Sebum | y=177 370x+91 073 | 0.999 6 | 75.7 | 13.9 | y=285 097x+223 774 | 0.999 3 | 73.2 | 11.7 |
| 停药后时间/d Time after withdrawal/d | 恩诺沙星残留总量/(μg·kg-1)Total enrofloxacin residues/(μg·kg-1) | |||
|---|---|---|---|---|
| 肌肉Muscle | 肝Liver | 肾Kidney | 皮脂Sebum | |
| 5 | 463.6±88.8 b | 287.7±92.1 a | 1 490.3±589.2 a | 6 578.3±2 099.9 a |
| 7 | 482.5±114.2 b | 225.6±52.1 a | 1 595.7±366.3 a | 5 326.2±2 711.5 ab |
| 10 | 516.2±160.4 b | 74.9±16.0 b | 1 453.4±364.9 a | 4 479.3±2 499.1 abc |
| 14 | 848.0±164.3 a | 75.4±27.6 b | 889.8±484.3 ab | 3 558.2±1 475.1 abc |
| 21 | 590.7±170.9 b | 42.2±9.27 b | 636.8±300.5 b | 1 644.5±496.0 c |
| 28 | 345.6±91.0 bc | 36.2±6.24 b | 382.9±170.1 b | 1 710.7±815.5 c |
| 42 | 196.1±71.3 c | 20.4±6.05 b | 245.8±149.5 b | 2 347.5±1 396.9 bc |
Table 5 Total enrofloxacin residues in different tissues of hens
| 停药后时间/d Time after withdrawal/d | 恩诺沙星残留总量/(μg·kg-1)Total enrofloxacin residues/(μg·kg-1) | |||
|---|---|---|---|---|
| 肌肉Muscle | 肝Liver | 肾Kidney | 皮脂Sebum | |
| 5 | 463.6±88.8 b | 287.7±92.1 a | 1 490.3±589.2 a | 6 578.3±2 099.9 a |
| 7 | 482.5±114.2 b | 225.6±52.1 a | 1 595.7±366.3 a | 5 326.2±2 711.5 ab |
| 10 | 516.2±160.4 b | 74.9±16.0 b | 1 453.4±364.9 a | 4 479.3±2 499.1 abc |
| 14 | 848.0±164.3 a | 75.4±27.6 b | 889.8±484.3 ab | 3 558.2±1 475.1 abc |
| 21 | 590.7±170.9 b | 42.2±9.27 b | 636.8±300.5 b | 1 644.5±496.0 c |
| 28 | 345.6±91.0 bc | 36.2±6.24 b | 382.9±170.1 b | 1 710.7±815.5 c |
| 42 | 196.1±71.3 c | 20.4±6.05 b | 245.8±149.5 b | 2 347.5±1 396.9 bc |
| 停药后时间/d Time after withdrawal/d | 恩诺沙星残留总量/(μg·kg-1)Total enrofloxacin residues/(μg·kg-1) | |||
|---|---|---|---|---|
| 肌肉Muscle | 肝Liver | 肾Kidney | 皮脂Sebum | |
| 5 | 371.1±166.1 ab | 230.0±85.0 a | 1 509.1±729.0 a | 5 525.0±786.3 ab |
| 7 | 337.4±201.0 ab | 212.8±116.0 ab | 1 649.3±962.4 a | 5 341.5±1 582.0 abc |
| 10 | 383.8±169.3 ab | 113.4±40.5 bc | 1 578.0±551.4 a | 6 404.1±905.6 a |
| 14 | 508.9±175.6 a | 62.8±32.3 c | 623.6±317.8 b | 4 692.3±1 813.5 abc |
| 21 | 317.6±118.3 b | 69.0±48.2 c | 339.7±218.6 b | 3 185.3±1 335.1 cd |
| 28 | 183.0±78.2 b | 30.3±13.6 c | 213.3±140.0 b | 3 350.2±609.5 bcd |
| 42 | 139.2±50.0 b | 11.4±3.2 c | 223.8±123.1 b | 2 452.7±359.6 d |
Table 6 Total enrofloxacin residues in different tissues of roosters
| 停药后时间/d Time after withdrawal/d | 恩诺沙星残留总量/(μg·kg-1)Total enrofloxacin residues/(μg·kg-1) | |||
|---|---|---|---|---|
| 肌肉Muscle | 肝Liver | 肾Kidney | 皮脂Sebum | |
| 5 | 371.1±166.1 ab | 230.0±85.0 a | 1 509.1±729.0 a | 5 525.0±786.3 ab |
| 7 | 337.4±201.0 ab | 212.8±116.0 ab | 1 649.3±962.4 a | 5 341.5±1 582.0 abc |
| 10 | 383.8±169.3 ab | 113.4±40.5 bc | 1 578.0±551.4 a | 6 404.1±905.6 a |
| 14 | 508.9±175.6 a | 62.8±32.3 c | 623.6±317.8 b | 4 692.3±1 813.5 abc |
| 21 | 317.6±118.3 b | 69.0±48.2 c | 339.7±218.6 b | 3 185.3±1 335.1 cd |
| 28 | 183.0±78.2 b | 30.3±13.6 c | 213.3±140.0 b | 3 350.2±609.5 bcd |
| 42 | 139.2±50.0 b | 11.4±3.2 c | 223.8±123.1 b | 2 452.7±359.6 d |
Fig.1 Fitted elimination curves of enrofloxacin residues in different tissues of hens A, Muscle; B, Liver; C, Kidney; D, Sebum; MRL, Maximum residue limit; Y-axis values are lg-transformed. The same as below.
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