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浙江大学学报(农业与生命科学版)  2021, Vol. 47 Issue (1): 127-134    DOI: 10.3785/j.issn.1008-9209.2020.03.241
动物科学与动物医学     
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
张静(),周倩,高玉时(),唐修君,陆俊贤,马丽娜,陈大伟,唐梦君
江苏省家禽科学研究所,江苏 扬州 225125
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
 全文: PDF(1127 KB)   HTML
摘要:

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    
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 words: florfenicol    florfenicol amine    egg    residue depletion    high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)
收稿日期: 2020-03-24 出版日期: 2021-03-09
CLC:  S  
基金资助: 江苏省现代农业重点及面上项目(BE2018363);江苏省属公益类科研院所自主科研经费(BM2018026);国家自然科学基金青年科学基金(31700005);江苏省扬州市重点研发计划(社会发展)项目(YZ2020060);江苏省现代农业产业技术体系建设专项资金(JATS〔2020〕359)
通讯作者: 高玉时     E-mail: zhangjing9143@126.com;gaoys100@sina.com
作者简介: 张静(https://orcid.org/0000-0003-4772-7648),E-mail:zhangjing9143@126.com
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引用本文:

张静,周倩,高玉时,唐修君,陆俊贤,马丽娜,陈大伟,唐梦君. 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[J]. 浙江大学学报(农业与生命科学版), 2021, 47(1): 127-134.

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.

链接本文:

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

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
表1  氟苯尼考和氟苯尼考胺在全蛋、蛋黄和蛋清中的回收率和精密度

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
表2  鸡蛋中氟苯尼考残留量 (μg/kg)

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
表3  鸡蛋中氟苯尼考胺残留量 (μg/kg)

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
表4  鸡蛋中氟苯尼考与氟苯尼考胺的总残留量 (μg/kg)
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