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加速溶剂萃取/超高效液相色谱-荧光法检测鸽蛋和鹌鹑蛋中氟苯尼考和氟苯尼考胺残留

刁志祥 王波 张培杨 王旭堂 谢恺舟 赵霞

刁志祥,王波,张培杨,等. 加速溶剂萃取/超高效液相色谱-荧光法检测鸽蛋和鹌鹑蛋中氟苯尼考和氟苯尼考胺残留 [J]. 福建农业学报,2019,34(11):1315−1322. doi: 10.19303/j.issn.1008-0384.2019.11.012
引用本文: 刁志祥,王波,张培杨,等. 加速溶剂萃取/超高效液相色谱-荧光法检测鸽蛋和鹌鹑蛋中氟苯尼考和氟苯尼考胺残留 [J]. 福建农业学报,2019,34(11):1315−1322. doi: 10.19303/j.issn.1008-0384.2019.11.012
DIAO Z X, WANG B, ZHANG P Y, et al. ASE/UHPLC-FLD Determination of Florfenicol and Florfenicol Amine Residues in Pigeon and Quail Eggs [J]. Fujian Journal of Agricultural Sciences,2019,34(11):1315−1322. doi: 10.19303/j.issn.1008-0384.2019.11.012
Citation: DIAO Z X, WANG B, ZHANG P Y, et al. ASE/UHPLC-FLD Determination of Florfenicol and Florfenicol Amine Residues in Pigeon and Quail Eggs [J]. Fujian Journal of Agricultural Sciences,2019,34(11):1315−1322. doi: 10.19303/j.issn.1008-0384.2019.11.012

加速溶剂萃取/超高效液相色谱-荧光法检测鸽蛋和鹌鹑蛋中氟苯尼考和氟苯尼考胺残留

doi: 10.19303/j.issn.1008-0384.2019.11.012
基金项目: 国家现代农业产业技术体系建设专项(CARS-41-G23);扬州大学"高端人才支持计划"项目(201801)
详细信息
    作者简介:

    刁志祥(1996−),男,硕士,研究方向:畜产品品质与安全(E-mail:1178257857@qq.com

    通讯作者:

    谢恺舟(1964−),男,博士,研究员,研究方向:畜产品品质、安全与兽药残留检测方法(E-mail:yzxkz168@163.com

  • 中图分类号: S 859.79+6

ASE/UHPLC-FLD Determination of Florfenicol and Florfenicol Amine Residues in Pigeon and Quail Eggs

  • 摘要:   目的  建立鸽蛋和鹌鹑蛋中尼考(florfenicol,FF)及其主要代谢产物氟苯尼考胺(florfenicol amine,FFA)残留检测的加速溶剂萃取/超高效液相色谱-荧光检测(ASE/UPLC-FLD)法,为动物源性食品中FF和FFA残留检测提供新的安全可靠的方法。  方法  采用加速溶剂萃取(ASE)法,用乙腈﹕氨水(98﹕2,V/V)为提取剂萃取样品,用乙腈饱和的正己烷去脂进行纯化,使用由0.005 mol·L-1 NaH2PO4、0.003 mol·L−1十二烷基硫酸钠和0.05%三甲胺组成的流动相供UPLC-FLD检测。  结果  鸽蛋和鹌鹑蛋中FF和FFA在定量限(LOQ)~400 μg·kg−1范围内,目标物的峰面积与其浓度均呈现良好的线性关系,相关系数(R2)均大于0.999 2。样品在LOQ、50.0、100.0、200.0 μg·kg−1的加标水平下的平均回收率为84.69%~98.04%,相对标准偏差(RSD)均低于3.7%。鸽蛋中FF的检测限(LOD)和LOQ为4.8 μg·kg−1和11.2 μg·kg−1,FFA的LOD和LOQ为1.9 μg·kg−1和4.8 μg·kg−1;鹌鹑蛋中FF的LOD和LOQ为4.7 μg·kg−1和10.6 μg·kg−1,FFA的LOD和LOQ为1.8 μg·kg−1和4.6 μg·kg−1  结论  该方法快速、简单、灵敏度高,适合禽蛋中FF及其代谢产物FFA的检测。
  • 图  1  标准品、空白鸽蛋/鹌鹑蛋、空白鸽蛋/鹌鹑蛋样品添加标准品(FF和FFA 50 μg·kg−1)色谱

    注:A,氟苯尼考和氟苯尼考胺标准品(50.0 μg·kg−1)色谱图;B,空白鸽蛋色谱图;C,加标鸽蛋样品色谱图;D,空白鹌鹑蛋色谱图;E,加标鹌鹑蛋样品色谱图。

    Figure  1.  Chromatograms of standards, pigeon egg/quail egg blank, pigeon egg/quail egg spiked with 50.0 µg·kg−1 FF and FFA

    Note:A=Chromatogram of FF and FFA standards (50.0 µg·kg−1); B=Chromatogram of pigeon egg blank; C=Chromatogram of spiked pigeon egg samples; D=Chromatogram of quail egg blank; E=Chromatogram of spiked quail egg samples.

    图  2  空白鸽蛋基质中添加氟苯尼考和氟苯尼考胺标准曲线

    注:A,空白鸽蛋基质中添加氟苯尼考标准曲线;B,空白鸽蛋基质中添加氟苯尼考胺标准曲线。

    Figure  2.  Standard curves of FF and FFA in pigeon egg

    Note:A=Curve of FF standards in pigeon egg; B=Curve of FFA standards in pigeon egg.

    图  3  空白鹌鹑蛋基质中添加氟苯尼考和氟苯尼考胺标准曲线

    注:A,空白鹌鹑蛋基质中添加氟苯尼考标准曲线;B,空白鹌鹑蛋基质中添加氟苯尼考胺标准曲线。

    Figure  3.  Standard curves of FF and FFA in quail egg

    Note:A=Curve of FF standards in quail egg; B=Curve of FFA standards in quail egg.

    表  1  不同萃取剂对氟苯尼考和氟苯尼考胺提取回收率的影响

    Table  1.   FF and FFA recoveries by different solvents (单位:%)

    分析物
    Analyte
    基质
    Matrix
    萃取剂乙腈氨水 Extraction reagent acetonitrile-ammonia
    991 982 973 964 955
    氟苯尼考
    FF
    鸽蛋
    Pigeon egg
    92.28±2.41 93.12±1.95 83.82±1.88 76.12±3.01 61.00±2.19
    鹌鹑蛋
    Quail egg
    92.73±2.23 94.24±2.47 86.24±2.49 74.48±2.41 68.53±2.48
    氟苯尼考胺
    FFA
    鸽蛋
    Pigeon egg
    88.23±2.24 96.32±2.14 86.53±2.70 73.09±2.13 64.82±2.27
    鹌鹑蛋
    Quail egg
    86.46±1.79 92.96±1.92 84.65±2.51 76.20±1.92 70.38±1.84
    下载: 导出CSV

    表  2  空白鸽蛋中FF和FFA添加回收率和精密度(n=6)

    Table  2.   Recovery and precision of determinations on pigeon egg spiked with FF and FFA (n=6)

    分析物
    Analyte
    添加质量比
    Adding level/(μg·kg−1
    回收率
    Recovery/%
    相对标准偏差
    RSD/%
    日内相对标准偏差
    Intra-day RSD/%
    日间相对标准偏差
    Inter-day RSD/%
    氟苯尼考
    FF
    11.2a 85.33±2.39 2.80 2.96 3.15
    50 96.42±2.10 2.18 3.84 4.52
    100b 98.04±3.63 3.70 3.25 4.97
    200 97.93±2.56 2.61 2.94 3.31
    氟苯尼考胺 FFA 4.8a 84.69±1.84 2.17 3.42 4.43
    50 94.08±2.43 2.58 2.70 3.06
    100.0b 95.14±2.90 3.05 3.86 5.18
    200 96.82±1.73 1.79 2.21 3.60
    注:a.定量限;b. 最高残留限量,表3同。
    Note:a=LOQ; b=Maximum residue limit. The same for Table 3.
    下载: 导出CSV

    表  3  空白鹌鹑蛋中FF和FFA添加回收率和精密度(n=6)

    Table  3.   Recovery and precision of determinations on quail egg spiked with FF and FFA (n=6)

    分析物
    Analyte
    添加质量比
    Adding level/(μg·kg−1
    回收率
    Recovery/%
    相对标准偏差
    RSD/%
    日内相对标准偏差
    Intra-day RSD/%
    日间相对标准偏差
    Inter-day RSD/%
    氟苯尼考
    FF
    10.6a 87.26±3.23 3.70 4.98 5.33
    50 95.73±2.14 2.24 2.65 3.58
    100b 95.36±2.91 3.05 3.73 4.49
    200 96.95±2.42 2.50 2.91 3.52
    氟苯尼考胺
    FFA
    4.6a 86.32±2.49 2.88 3.60 3.92
    50 96.73±2.75 2.84 4.13 5.43
    100.0b 95.62±3.21 3.36 3.54 5.62
    200 96.84±3.36 3.47 4.86 5.84
    下载: 导出CSV
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  • 收稿日期:  2019-07-13
  • 修回日期:  2019-10-04
  • 刊出日期:  2019-11-01

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