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Journal of Zhejiang University (Agriculture and Life Sciences)  2021, Vol. 47 Issue (1): 127-134    DOI: 10.3785/j.issn.1008-9209.2020.03.241
Animal sciences & veterinary medicine     
Residue depletion laws of florfenicol and its metabolite florfenicol amine in eggs
Jing ZHANG(),Qian ZHOU,Yushi GAO(),Xiujun TANG,Junxian LU,Lina MA,Dawei CHEN,Mengjun TANG
Jiangsu Institute of Poultry Sciences, Yangzhou 225125, Jiangsu, China
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Abstract  

A study on florfenicol (FF) and florfenicol amine (FFA) residue depletion raws was conducted in eggs. After the chickens were administered successively florfenicol (FF) powder of 15 mg/kg (prevention group) and 30 mg/kg (treatment group) of body mass in the form of premix for 5 d, the eggs of each group were collected at administration period and 1, 2, 3, 5, 7, 10, 12, 15, 18 d at withdrawal period. Then FF and FFA residues of egg, egg yolk and egg white were detected using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The results showed that the limits of detection (LOD) of FF and FFA in egg, egg yolk and egg white were 2 μg/kg, and the limits of quantitation (LOQ) were 5 μg/kg. The average recoveries were in the range of 78.9%-105.0% when the egg samples were added with FF in the range of 1.0-5.0 μg/kg, and the intraday precision and the interday precision was 2.22%-4.22% and 4.22%-6.54%, respectively. The peak values of FF residues (520.70, 797.12 μg/kg) of egg white in prevention group and treatment group, respectively, were higher than those of egg yolk (285.96, 442.40 μg/kg), while the peak values of FFA residue (218.40, 646.14 μg/kg) of egg yolk in prevention group and treatment group, respectively, were higher than those of egg white (87.36, 36.89 μg/kg). The elimination rates of FF and FFA in egg white were faster than those in egg yolk. FF and FFA residues and their total residues were positively correlated with the dosage. FF and FFA mainly existed in the egg yolk, and FF mainly existed in the egg white. The FF residual time of egg yolk in different dosage groups was 18 d.



Key wordsflorfenicol      florfenicol amine      egg      residue depletion      high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)     
Received: 24 March 2020      Published: 09 March 2021
CLC:  S  
Corresponding Authors: Yushi GAO     E-mail: zhangjing9143@126.com;gaoys100@sina.com
Cite this article:

Jing ZHANG,Qian ZHOU,Yushi GAO,Xiujun TANG,Junxian LU,Lina MA,Dawei CHEN,Mengjun TANG. Residue depletion laws of florfenicol and its metabolite florfenicol amine in eggs. Journal of Zhejiang University (Agriculture and Life Sciences), 2021, 47(1): 127-134.

URL:

http://www.zjujournals.com/agr/10.3785/j.issn.1008-9209.2020.03.241     OR     http://www.zjujournals.com/agr/Y2021/V47/I1/127


氟苯尼考及其代谢物氟苯尼考胺在鸡蛋中的残留消除规律

本试验旨在研究氟苯尼考及其代谢物氟苯尼考胺在鸡蛋中的残留消除规律。预防组和治疗组蛋鸡分别按体质量以15和30 mg/kg剂量预拌料方式给予氟苯尼考粉药物,连续5 d,分别收集给药期和停药后第1、2、3、5、7、10、12、15、18天的各组鸡蛋,测定全蛋、蛋黄和蛋清中氟苯尼考和氟苯尼考胺的残留量。结果表明:全蛋、蛋清和蛋黄中氟苯尼考和氟苯尼考胺的检出限均为2 μg/kg,定量限均为5 μg/kg。鸡蛋样品在氟苯尼考添加水平为1.0~5.0 μg/kg时平均回收率为78.9%~105.0%,日内精密度为2.22%~4.22%,日间精密度为4.22%~6.54%。停药后,氟苯尼考在预防组和治疗组蛋清中的残留量峰值(520.70、797.12 μg/kg)高于蛋黄(285.96、442.40 μg/kg),氟苯尼考胺在蛋黄中的残留量峰值(218.40、646.14 μg/kg)高于蛋清(87.36、36.89 μg/kg),氟苯尼考和氟苯尼考胺在蛋清中的消除速率均快于蛋黄。氟苯尼考和氟苯尼考胺残留量及其总残留量与给药剂量呈正相关,蛋黄中以氟苯尼考和氟苯尼考胺残留为主,蛋清中主要是氟苯尼考残留。不同剂量组蛋黄中氟苯尼考残留时间为18 d。


关键词: 氟苯尼考,  氟苯尼考胺,  鸡蛋,  残留消除,  高效液相色谱-串联质谱法 

分析物

Analyte

添加水平

Added level/(μg/kg)

回收率

Recovery/%

日内相对标准偏差

Intraday relative standard deviation/%

日间相对标准偏差

Interday relative standard deviation/%

全蛋

Egg

FF1.098.02.344.77
2.0104.03.515.33
5.0100.03.554.92
FFA1.0102.02.874.71
2.094.63.215.63
5.099.84.226.01

蛋黄

Egg

yolk

FF1.088.93.294.98
2.0101.04.216.32
5.0100.03.555.21
FFA1.078.92.784.73
2.093.02.224.65
5.095.63.215.01

蛋清

Egg

white

FF1.089.03.015.21
2.0105.02.984.55
5.0100.03.224.22
FFA1.087.84.026.54
2.098.93.875.98
5.097.12.985.21
Table 1 Recovery and precision of florfenicol (FF) and florfenicol amine (FFA) in egg, egg yolk and egg white

时期

Period

t/d15 mg/kg组 15 mg/kg group30 mg/kg组 30 mg/kg group

全蛋

Egg

蛋黄

Egg yolk

蛋清

Egg white

全蛋

Egg

蛋黄

Egg yolk

蛋清

Egg white

给药期

Administration period

13.75±2.7720.31±27.6224.53±1.1910.65±2.983.63±2.017.44±6.78
298.79±22.95145.54±11.49261.55±23.85226.92±16.7960.18±13.41408.57±11.51
3190.86±17.79104.59±24.69353.75±16.01460.89±14.52260.42±14.31882.05±22.00
4293.39±14.73142.70±11.17274.88±8.39481.47±17.98315.31±16.71394.24±21.40
5330.58±15.34148.00±25.34464.91±20.67665.10±28.16423.30±17.50782.39±21.54

停药期

Withdrawal period

1341.60±18.30281.89±16.95520.70±22.79758.41±24.58442.40±38.15797.12±25.92
2213.82±25.31285.96±17.62203.97±25.70412.67±21.66419.32±17.82229.67±15.77
3209.14±28.60230.19±28.89180.96±21.93220.62±34.58427.77±38.58124.80±22.64
5124.90±27.39201.18±21.5075.11±23.00164.72±29.05303.42±23.8535.84±30.69
770.07±15.3196.03±20.2621.64±6.1465.09±26.8096.11±12.502.23±2.24
1014.26±4.5023.73±3.56ND8.75±3.689.85±3.68ND
123.18±1.395.49±2.28ND1.51±0.343.40±1.36ND
15ND1.27±0.29NDND1.49±0.47ND
18NDNDNDNDNDND
Table 2 Residue of FF in eggs

时期

Period

t/d15 mg/kg组 15 mg/kg group30 mg/kg组 30 mg/kg group

全蛋

Egg

蛋黄

Egg yolk

蛋清

Egg white

全蛋

Egg

蛋黄

Egg yolk

蛋清

Egg white

给药期

Administration period

1ND12.10±15.39NDND2.41±1.35ND
213.60±2.3830.44±5.3012.17±2.1254.68±15.1617.14±6.9220.92±9.53
310.29±5.4324.98±10.939.99±4.3767.53±15.16114.00±15.4423.75±9.57
429.54±10.5662.16±21.7121.66±14.0699.38±24.27239.66±22.4018.69±12.23
538.40±10.6064.12±18.4321.43±13.83189.01±20.85405.01±30.8226.35±5.86

停药期

Withdrawal period

149.65±16.77218.40±8.2087.36±3.28285.48±16.24423.77±14.4236.89±14.35
254.36±19.63213.69±21.8385.48±8.73230.98±18.20470.35±23.6013.09±3.16
378.99±22.94214.22±29.1485.69±11.66123.32±35.73646.14±31.4621.31±16.20
544.44±24.88200.41±27.1866.70±38.17134.90±30.38454.83±23.4513.03±9.66
724.44±6.0749.52±17.4419.81±6.9848.11±27.0866.11±17.361.57±3.51
108.83±0.867.58±0.97ND7.38±0.957.05±1.90ND
126.25±0.304.30±0.57ND6.34±0.243.95±0.57ND
15ND3.03±0.16ND2.04±0.071.17±0.16ND
18NDNDNDNDNDND
Table 3 Residue of FFA in eggs

时期

Period

t/d15 mg/kg组 15 mg/kg group30 mg/kg组 30 mg/kg group

全蛋

Egg

蛋黄

Egg yolk

蛋清

Egg white

全蛋

Egg

蛋黄

Egg yolk

蛋清

Egg white

给药期

Administration period

13.75±2.7732.41±42.9424.53±1.1910.90±13.726.04±3.265.95±6.75
2112.39±24.94175.98±16.01273.72±23.19281.60±30.4677.32±20.22429.49±10.63
3201.16±20.69129.57±34.68363.75±13.50528.42±22.05374.42±21.42905.79±28.89
4322.93±21.75204.86±27.27296.54±21.25580.85±37.46554.97±31.35412.93±31.59
5368.98±25.10212.12±41.82486.34±29.68854.10±46.45828.31±25.33808.74±20.18

停药期

Withdrawal period

1391.25±22.44500.29±21.34608.06±25.481 043.89±20.66866.16±29.26834.01±21.69
2268.19±36.34499.65±36.74289.45±32.14643.65±34.52889.67±38.95242.76±16.09
3288.14±40.30444.41±46.81266.64±22.92343.94±69.981 073.91±29.57146.11±30.06
5169.34±49.91401.59±31.07141.82±44.45299.61±56.80758.25±38.9946.26±40.64
794.51±20.59145.55±29.4241.45±10.23113.21±53.42162.22±24.013.80±5.39
1023.09±5.1631.31±3.53ND16.12±3.7416.89±5.49ND
129.43±2.619.78±2.83ND7.85±0.207.35±1.66ND
15ND4.30±0.43ND6.95±0.754.66±0.54ND
18NDNDNDNDNDND
Table 4 Total residues of FF and FFA in eggs
[1]   FDA. Freedom of information summary original new animal drug application.
[2]   陈杖榴,邱银生,曾振灵.国内外兽药研制开发与市场动态.中国兽药杂志,2002,36(3):42-46.
CHEN Z L, QIU Y S, ZENG Z L. Development and market trends of veterinary drug at home and abroad. Chinese Journal of Veterinary Drug, 2002,36(3):42-46. (in Chinese)
[3]   中华人民共和国农业农村部.食品安全国家标准 食品中兽药最大残留限量:GB 31650—2019.北京:中国标准出版社,2019.
Ministry of Agriculture and Rural Affairs of the People’s Republic of China. National Food Safety Standard-Maximun Residue Limits for Veterinary Drugs in Foods: GB 316502019. Beijing: Standards Press of China, 2019. (in Chinese)
[4]   张静,高玉时,周倩,等.高效液相色谱-电喷雾电离串联质谱法测定鸡肉、鸡蛋中氯霉素、甲砜霉素和氟苯尼考药物残留量.食品安全质量检测学报,2017,8(6):2211-2219.
ZHANG J, GAO Y S, ZHOU Q, et al. Determination of chlorampheincol, thiamphenicol and florfenicol residues in chicken and egg by high performance liquid chromatography-electrospray ionization-tandem mass spectrometry. Journal of Food Safety and Quality, 2017,8(6):2211-2219. (in Chinese with English abstract)
[5]   曾勇,董文婷,龚波,等.超高效液相色谱-串联质谱法快速测定禽蛋中氯霉素、氟苯尼考及其代谢物残留.中国兽药杂志,2017,51(12):42-46. DOI:10.11751/ISSN.1002-1280.2017.12.08
ZENG Y, DONG W T, GONG B, et al. Rapid determination of chloramphenicol, florfenicol and its metabolites in poultry eggs by UPLC-MS/MS. Chinese Journal of Veterinary Drug, 2017,51(12):42-46. (in Chinese with English abstract)
doi: 10.11751/ISSN.1002-1280.2017.12.08
[6]   陈芩,章剑,胡洁,等.高效液相色谱法检测蛋及蛋制品中氟苯尼考残留量.现代农业科技,2018(3):259-260, 262.
CHEN Q, ZHANG J, HU J, et al. Detection of florfenicol residue in eggs and egg products by HPLC. Modern Agricultural Science and Technology, 2018(3):259-260, 262. (in Chinese with English abstract)
[7]   王波,赵霞,谢恺舟,等.鸽蛋中氯霉素甲砜霉素氟苯尼考及其代谢物氟苯尼考胺同时检测的超高效液相色谱-串联质谱法的建立.中国兽医科学,2019,49(3):393-402. DOI:10.16656/j.issn.1673-4696.2019.0050
WANG B, ZHAO X, XIE K Z, et al. Simultaneous determination of chloramphenicol, thiamphenicol, florfenicol and its metabolite florfenicol amine in pigeon eggs by UPLC-ESI/MS/MS. Chinese Veterinary Science, 2019,49(3):393-402. (in Chinese with English abstract)
doi: 10.16656/j.issn.1673-4696.2019.0050
[8]   卢运战.鸡组织中甲砜霉素和氟苯尼考残留的检测方法及消除规律.合肥:安徽农业大学,2007:22-28.
LU Y Z. The determination method of thiamphenicol and florfenicol residues and their elimination in chicken tissues. Hefei: Anhui Agricultural University, 2007:22-28. (in Chinese with English abstract)
[9]   李建成.氟苯尼考及其代谢物氟苯尼考胺在猪和鸡组织中检测方法及残留消除规律的研究.北京:中国农业大学,2007:59-74.
LI J C. The determination method of florfenicol and the metabolite florfenicol amine residues and their elimination in swine and broiler chicken tissue. Beijing: China Agricultural University, 2007:59-74. (in Chinese with English abstract)
[10]   王群,何玉英,李健.氟苯尼考在中国对虾体内消除规律的研究.中国海洋大学学报(自然科学版),2007,37(2):251-254. DOI:16441/j.cnki.hdxb.2007.02.014
WANG Q, HE Y Y, LI J. Elimination of florfenicol in Fenneropenaeus chinensis. Periodical of Ocean University of China, 2007,37(2):251-254. (in Chinese with English abstract)
doi: 16441/j.cnki.hdxb.2007.02.014
[11]   谢凯舟,张小杰,陈学森,等.氟苯尼考及其代谢物氟苯尼考胺在鸡肌肉中的残留消除规律.畜牧兽医学报,2012,43(8):1298-1305.
XIE K Z, ZHANG X J, CHEN X S, et al. Florfenicol and its metabolite florfenicol amine residue depletion in chicken muscle. Acta Veterinaria et Zootechnica Sinica, 2012,43(8):1298-1305. (in Chinese with English abstract)
[12]   孙泽祥,杨挺,鲍伟华,等.鸡组织中氟苯尼考和氟苯尼考胺代谢动力学研究.畜牧兽医科技信息,2009(8):21-23. DOI:10.3969/J.ISSN.1671-6027.2009.08.016
SUN Z X, YANG T, BAO W H, et al. Pharmacokinetics study of florfenicol and florfenicol amine in chicken tissue. Chinese Journal of Animal Husbandry and Veterinary Medicine, 2009(8):21-23. (in chinese)
doi: 10.3969/J.ISSN.1671-6027.2009.08.016
[13]   宋志超,张崇威,陈蔷,等.氟苯尼考注射液在鸡体内残留消除研究.中国兽药杂志,2018,52(12):35-43. DOI:10.11751/ISSN.1002-1280.2018.12.06
SONG Z C, ZHANG C W, CHEN Q, et al. Residue depletion study of florfenicol injection in chicken. Chinese Journal of Veterinary Drug, 2018,52(12):35-43. (in Chinese with English abstract)
doi: 10.11751/ISSN.1002-1280.2018.12.06
[14]   刘崇万,孟勇,朱晓华,等.池塘养殖模式下氟苯尼考及其代谢产物在斑点叉尾鮰体内及养殖环境中残留消除及迁移行为.中国渔业质量与标准,2019,9(5):30-40. DOI:10.3969/j.issn.2095-1833.2019.05.005
LIU C W, MENG Y, ZHU X H, et al. Elimination and migration of florfenicol and its metabolic residues in Letaurus punetaus and aquaculture environment under pond conditions. Chinese Fishery Quality and Standards, 2019,9(5):30-40. (in Chinese with English abstract)
doi: 10.3969/j.issn.2095-1833.2019.05.005
[15]   全国认证认可标准化技术委员会.实验室质量控制规范 食品理化检测:GB/T 27404—2008.北京:中国标准出版社,2008.
National Certification and Accreditation Standardization Technical Committee. Criterion on Quality Control of Laboratories-Chemical Testing of Food: GB/T 27404—2008. Beijing: Standards Press of China, 2008. (in Chinese)
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