Determination of Spiramycin Residue in Pork by Synchronous Fluorimetry with Sulphuric Acid Oxidation

doi:10.3969/j.issn.1000-1565.2010.01.014

Abstract

Abstract: Nonfluorescent spiramycin can be oxidized into fluorescent substance with concentrated sulfuric acid. When the synchronous fluorescence spectra are scanned from 400 nm to 600 nm at the emission and excition wavelength difference of 25 nm, the maximum fluorescence intensity can be measured at 494 nm. A new assay is developed to determine spiramycin residue based on the principle. Under the optimum condition, linear dynamic range is 0.02-4 mg/L; detection limit is 0.33 μg/kg; the recoveries of spiked sample is between 100.31% and 107.78%. The method has been successfully applied to the determination of spiramycin residue in pork.

Key words: spiramycin, sulfuric acid, oxidation, synchronous fluorimetry

CLC Number:

O657.31

ZHANG Yan,CHEN Guan-hua,HAO Qing-hong,CHEN Zhi-min,GUO Yun-xia. Determination of Spiramycin Residue in Pork by Synchronous Fluorimetry with Sulphuric Acid Oxidation[J]. Journal of Hebei University (Natural Science Edition), 2010, 30(1): 64-68.

References

[1] 王海涛, 张睿, 段宏安, 姚燕林, WANG Hai-tao, ZHANG Rui, DUAN Hong-an, YAO Yan-lin. 高效液相色谱法同步检测牛奶中替米考星、泰乐菌素和螺旋霉素残留量 [J]. 分析试验室 2008.doi:10.3969/j.issn.1000-0720.2008.07.027
[2] 杨方, 李耀平, 方宇, 刘正才, YANG Fang, LI Yao-ping, FANG Yu, LIU Zheng-cai. 高效液相色谱法同时检测水产品中螺旋霉素与泰乐菌素药物残留 [J]. 理化检验-化学分册 2007.doi:10.3321/j.issn:1001-4020.2007.04.007
[3] 侯芳菲, 陈冠华, HOU Fang-fei, CHEN Guan-hua. 荧光分光光度法测定梨中残留双甲脒 [J]. 河北大学学报（自然科学版） 2006.doi:10.3969/j.issn.1000-1565.2006.02.016
[4] 赵燕燕, 苏芳, 王翠玲, 姜明明, 白洁, 陈春生, 张向飞, ZHAO Yan-yan, SU Fang, WANG Cui-ling, JIANG Ming-ming, BAI Jie, CHEN Chun-sheng, ZHANG Xiang-fei. 同步荧光-双波长法同时测定血浆中儿茶酚胺类神经递质 [J]. 河北大学学报（自然科学版） 2008.doi:10.3969/j.issn.1000-1565.2008.01.016
[5] 国家质量监督检验检疫总局进出口食品安全局. 兽药残留限量查询 [EB/OL]. http://www.tbt-sps.gov.cn/foodsafe/xlbz/Pages/veterinary.aspx 2009.
[6] 国家质量监督检验检疫总局进出口食品安全局. 日本肯定列表 [EB/OL]. http://www.tbt-sps.gov.cn/foodsafe/xlbz/Pages/japan.aspx 2009.
[7] 中华人民共和国农业部. 动物性食品中兽药最高残留限量 [EB/OL]. http://www.agri.gov.cn/xumugb/99-2-2.htm 2009.
[8] Naoto Furusawa. Normal-phase high-performance liquid chromatographic determination of spiramycin in eggs and chicken [J]. Talanta: The International Journal of Pure and Applied Analytical Chemistry 1999, 2(2).
[9] Brambilla G. Identification and quantification method of spiramycin and tylosin in feedingstuffs with HPLC-UV/DAD at 1ppm level. [J]. Journal of Pharmaceutical and Biomedical Analysis: An International Journal on All Drug-Related Topics in Pharmaceutical, Biomedical and Clinical Analysis 2004, 2(2).
[10] Maria Jose Gonzalez de la Huebra, Ursula Vincent, Guy Bordin, Adela Rosa Rodriguez. Characterisation of dirithromycin and spriamycin using high performance liquid chromatography and direct infusion mass spectrometry [J]. Analytica chimica acta 2004, 2(2).
[11] Sagan C, Salvador A, Dubreuil D, Poulet PP, Duffaut D, Brumpt I. Simultaneous determination of metronidazole and spiramycin I in human plasma, saliva and gingival crevicular fluid by LC-MS/MS. [J]. Journal of Pharmaceutical and Biomedical Analysis: An International Journal on All Drug-Related Topics in Pharmaceutical, Biomedical and Clinical Analysis 2005, 2(2).
[12] ZHANG Shuhong, HUANG Xian, YAO Naisheng. Preparation of monodisperse porous polymethacrylate microspheres and their application in the capillary electrochromatography of macrolide antibiotics [J]. Journal of Chromatography A 2002, 948(1-2).
[13] 周森麟, 谭明. 大量体液样品中螺旋霉素的效价测定 [J]. 中国医院药学杂志 1994, 14(08).
[14] 沈克文, 王绪明, 韩永平. 实用药物分离鉴定手册 [M]. 北京:人民军医出版社 1986.
[15] 陈奎, 孙旭峰, 吴剑鸣. 硫酸颜色反应用于乙酸螺旋霉素的测定 [J]. 分析化学 1998, 26(12).
[16] 吴剑鸣. 硫酸颜色反应用于乙酰螺旋霉素的荧光法测定 [J]. 1998.