SNW-1 Magnetic Solid Phase Extraction for HPLC Detection of Sulfonamides Residue in Milk

NING Qian; CHEN Yu; YAN Zhiming

doi:10.19303/j.issn.1008-0384.2020.10.014

Volume 35 Issue 10

Oct. 2020

Turn off MathJax

Article Contents

Article Navigation > Fujian Journal of Agricultural Sciences > 2020 > 35(10): 1154-1161

NING Q, CHEN Y, YAN Z M. SNW-1 Magnetic Solid Phase Extraction for HPLC Detection of Sulfonamides Residue in Milk [J]. Fujian Journal of Agricultural Sciences，2020，35（10）：1154−1161 doi: 10.19303/j.issn.1008-0384.2020.10.014

Citation:

NING Q, CHEN Y, YAN Z M. SNW-1 Magnetic Solid Phase Extraction for HPLC Detection of Sulfonamides Residue in Milk [J]. Fujian Journal of Agricultural Sciences，2020，35（10）：1154−1161 doi: 10.19303/j.issn.1008-0384.2020.10.014

Citation:

PDF( 1654 KB)

SNW-1 Magnetic Solid Phase Extraction for HPLC Detection of Sulfonamides Residue in Milk

doi: 10.19303/j.issn.1008-0384.2020.10.014

NING Qian^1
,,
CHEN Yu²,
YAN Zhiming^{2
,
,}

1.
Jinshan College, Fujian Agriculture and Forestry University, Fuzhou, Fujian　350002, China
2.
College of Food Science, Fujian Agriculture and Forestry University, Fuzhou, Fujian　350002, China

Received Date: 2019-09-02
Rev Recd Date: 2020-01-29
Publish Date: 2020-10-28

Abstract

Abstract

Objective Fe₃O₄@SNW-1 was prepared as an adsorbent in the magnetic solid phase extraction (MSPE) to pre-treat samples for HPLC determination on sulfonamides (SAs) in milk. Method A magnetic covalent organic framework (COF) material, Fe₃O₄@SNW-1, was hydrothermally synthesized to serve as the adsorbent in MSPE for the sample pretreatment. Parameters for the pretreatment, including adsorbent usage, adsorption duration, eluent selection, and elution time that affected the extract recovery, were optimized. HPLC was used to evaluate and determine the validity of the methodology. Result The optimized MSPE applying 2.0 mL ammonia-methanol (5 ∶ 95, V/V) as elution solvent, 60s for desorption, 4.0 mg of Fe₃O₄@SNW-1 as adsorbent, 120 s for adsorption at pH 6.0 to achieve linearities in the ranges between 10 ng·mL⁻¹ and 100 ng·mL⁻¹ on detecting 5 different SAs with correlation coefficients greater than 0.995. The HPLC detection limit on the SAs was 1.7-2.7 ng·mL⁻¹. The daytime RSDs of 5 extraction replicates on the SAs (50 ng·mL⁻¹ each) were 2.8–4.7%. The recovery rates on the SAs varied from 72.0% to 95.0%. Conclusion The proposed HPLC method with the MSPE sample pretreatment was convenient, rapid, specific, and effective for the determination of trace amounts of SA residues in milk.
- Covalent organic frameworks,
- sample pretreatment,
- magnetic solid phase extraction,
- milk,
- sulfonamides

FullText(HTML)

References(28)

References

[1]	赵超敏, 岳振峰, 吴晖, 等. 液相色谱-串联质谱法测定牛奶中4种雌激素残留 [J]. 现代食品科技, 2014, 30(6):244−249. ZHAO C M, YUE Z F, WU H, et al. Determination of four estrogens residues in milk samples by liquid chromatography-tandem mass spectrometry [J]. Modern Food Science & Technology, 2014, 30(6): 244−249.(in Chinese)
[2]	晏利芝, 赵永彪, 富玉, 等. 超高效液相色谱-串联质谱法同时测定猪肉中β-受体激动剂、喹诺酮类和磺胺类兽药残留量 [J]. 分析试验室, 2011, 30(1):84−86. doi: 10.3969/j.issn.1000-0720.2011.01.024 YAN L Z, ZHAO Y B, FU Y, et al. Simultaneous determination of β-agonist, quinolones and sulfonamides residues in pork by ultra performance liquid chromatography-electrosp ray ionization tandem mass spectrometry [J]. Chinese Journal of Analysis Laboratory, 2011, 30(1): 84−86.(in Chinese) doi: 10.3969/j.issn.1000-0720.2011.01.024
[3]	王泽岚, 周艳芬, 孟哲, 等. 核壳聚苯胺选择性磁性固相萃取-高效液相色谱-质谱法测定牛奶中痕量磺胺类药物 [J]. 分析化学, 2019, 47(1):119−128. WANG Z L, ZHOU Y F, MENG Z, et al. Determination of trace sulfonamides antibiotics in milk using polyaniline silicon magnetic composite selective magnetic solid phase extraction combined with high performance liquid chromatography-mass spectrometry [J]. Chinese Journal of Analytical Chemistry, 2019, 47(1): 119−128.(in Chinese)
[4]	中华人民共和国国家标准. 食品卫生微生物学检验鲜乳中抗生素残留量检测: GB/T 32738-2016 [S]. 北京: 中国标准出版社, 2008.
[5]	吴瑕, 张兰威. 牛乳中抗生素残留及其检测方法的研究进展 [J]. 食品与发酵工业, 2004, 30(7):112−116. doi: 10.3321/j.issn:0253-990X.2004.07.027 WU X, ZHANG L W. Development of methods for detection of antibiotics residues in milk [J]. Food and Fermentation Industries, 2004, 30(7): 112−116.(in Chinese) doi: 10.3321/j.issn:0253-990X.2004.07.027
[6]	段婕, 李兴华, 刘坤, 等. 高效液相色谱-化学发光法检测牛奶中磺胺类药物残留 [J]. 分析化学, 2017, 45(7):1012−1018. doi: 10.11895/j.issn.0253-3820.170110 DUAN J, LI X H, LIU K, et al. Determination of sulfonamide residues in milk by high performance liquid chromatography-chemiluminescence method [J]. Chinese Journal of Analytical Chemistry, 2017, 45(7): 1012−1018.(in Chinese) doi: 10.11895/j.issn.0253-3820.170110
[7]	李龙飞, 苏敏, 石晓蕾, 等. 磁性固相萃取技术在牛奶中兽药残留检测的应用发展现状 [J]. 乳业科学与技术, 2013, 36(5):35−38. LI L F, SU M, SHI X L, et al. Progress in applications of magnetic solid phase extraction in detection of veterinary drugs residuals in milk [J]. Journal of Dairy Science and Technology, 2013, 36(5): 35−38.(in Chinese)
[8]	王翔, 邓晓军, 宋国新, 等. 食品中磺胺类兽药残留前处理技术的研究进展 [J]. 食品科学, 2009, 30(7):254−257. doi: 10.3321/j.issn:1002-6630.2009.07.059 WANG X, DENG X J, SONG G X, et al. Research progress on pretreatment technologies of sulfonamides residues in food for their determination [J]. Food Science, 2009, 30(7): 254−257.(in Chinese) doi: 10.3321/j.issn:1002-6630.2009.07.059
[9]	COMBS M T, ASHRAF-KHORASSANI M, TAYLOR L T. Comparison of supercritical CHF₃ and CO₂ for extraction of sulfonamides from various food matrices [J]. Analytical Chemistry, 1996, 68(24): 4507−4511. doi: 10.1021/ac960643q
[10]	ARANCIBIA V, VALDERRAMA M, RODRIGUEZ P, et al. Quantitative extraction of sulfonamides in meats by supercritical methanol-modified carbon dioxide: A foray into real-world sampling [J]. Journal of Separation Science, 2003, 26(18): 1710−1716. doi: 10.1002/jssc.200301501
[11]	LU K H, CHEN C Y, LEE M R. Trace determination of sulfonamides residues in meat with a combination of solid-phase microextraction and liquid chromatography-mass spectrometry [J]. Talanta, 2007, 72(3): 1082−1087. doi: 10.1016/j.talanta.2007.01.022
[12]	BALAKRISHNAN V K, TERRY K A, TOITO J. Determination of sulfonamide antibiotics in wastewater: A comparison of solid phase microextraction and solid phase extraction methods [J]. Journal of Chromatography A, 2006, 1131(1/2): 1−10.
[13]	XUE R, GUO H, WANG T, et al. Fluorescence properties and analytical applications of covalent organic frameworks [J]. Analytical Methods, 2017, 9(25): 3737−3750. doi: 10.1039/C7AY01261F
[14]	QI F F, QIAN L L, LIU J J, et al. A high-throughput nanofibers mat-based micro-solid phase extraction for the determination of cationic dyes in wastewater [J]. Journal of Chromatography. A, 2016, 1460: 24−32. doi: 10.1016/j.chroma.2016.07.020
[15]	魏文英, 方键, 孔海宁, 等. 金属有机骨架材料的合成及应用 [J]. 化学进展, 2005, 17(6):1110−1115. doi: 10.3321/j.issn:1005-281X.2005.06.023 WEI W Y, FANG J, KONG H N, et al. Synthesis and applications for materials of metallorganic frameworks [J]. Progress in Chemistry, 2005, 17(6): 1110−1115.(in Chinese) doi: 10.3321/j.issn:1005-281X.2005.06.023
[16]	吴科盛, 许恒毅, 郭亮, 等. 磁性固相萃取在检测分析中的应用研究进展 [J]. 食品科学, 2011, 32(23):317−320. WU K S, XU H Y, GUO L, et al. Progress in applications of magnetic solid phase extraction in detection and analysis [J]. Food Science, 2011, 32(23): 317−320.(in Chinese)
[17]	王露, 汪怡, 杭学宇, 等. 磁性高交联聚苯乙烯-纳米Fe₃O₄的制备及其在牛奶中磺胺类药物检测中的应用 [J]. 分析试验室, 2016, 35(9):1052−1055. WANG L, WANG Y, HANG X Y, et al. Magnetic solid phase extraction based on magnetic hypercross linked polystyrene for determination of sulfonamides in milk samples [J]. Chinese Journal of Analysis Laboratory, 2016, 35(9): 1052−1055.(in Chinese)
[18]	TOLMACHEVA V V, APYARI V V, FURLETOV A A, et al. Facile synthesis of magnetic hypercrosslinked polystyrene and its application in the magnetic solid-phase extraction of sulfonamides from water and milk samples before their HPLC determination [J]. Talanta, 2016, 152: 203−210. doi: 10.1016/j.talanta.2016.02.010
[19]	李路路, 刘帅, 章琴, 等. 共价有机框架材料研究进展 [J]. 物理化学学报, 2017, 33(10):1960−1977. doi: 10.3866/PKU.WHXB201705191 LI L L, LIU S, ZHANG Q, et al. Advances in covalent organic frameworks [J]. Acta Physico-Chimica Sinica, 2017, 33(10): 1960−1977.(in Chinese) doi: 10.3866/PKU.WHXB201705191
[20]	李文超, 王永花, 孙成, 等. 分子印迹技术与固相微萃取技术联用的研究进展 [J]. 环境化学, 2011, 30(9):1663−1671. LI W C, WANG Y H, SUN C, et al. The development of molecularly imprinted technique coupled with solid phase microextraction [J]. Environmental Chemistry, 2011, 30(9): 1663−1671.(in Chinese)
[21]	GUO J X, QIAN H L, ZHAO X, et al. In situ room-temperature fabrication of a covalent organic framework and its bonded fiber for solid-phase microextraction of polychlorinated biphenyls in aquatic products [J]. Journal of Materials Chemistry A, 2019, 7(21): 13249−13255. doi: 10.1039/C9TA02974E
[22]	LIU L, MENG W K, ZHOU Y S, et al. β-Ketoenamine-linked covalent organic framework coating for ultra-high-performance solid-phase microextraction of polybrominated diphenyl ethers from environmental samples [J]. Chemical Engineering Journal, 2019, 356: 926−933. doi: 10.1016/j.cej.2018.09.081
[23]	QIAN H L, YANG C X, WANG W L, et al. Advances in covalent organic frameworks in separation science [J]. Journal of Chromatography. A, 2018, 1542: 1−18. doi: 10.1016/j.chroma.2018.02.023
[24]	OLGUN C E, MUYAN M. SNW₁ (SNW domain containing 1) [J]. Atlas of Genetics and Cytogenetics in Oncology and Haematology, 2018(6): 233−235. doi: 10.4267/2042/68909
[25]	IBARRA I S, MIRANDA J M, RODRIGUEZ J A, et al. Magnetic solid phase extraction followed by high-performance liquid chromatography for the determination of sulphonamides in milk samples [J]. Food Chemistry, 2014, 157: 511−517. doi: 10.1016/j.foodchem.2014.02.069
[26]	SHI P Z, YE N S. Magnetite–graphene oxide composites as a magnetic solid-phase extraction adsorbent for the determination of trace sulfonamides in water samples [J]. Analytical Methods, 2014, 6(24): 9725−9730. doi: 10.1039/C4AY02027H
[27]	LI Y Z, WU X W, LI Z Q, et al. Fabrication of CoFe₂O₄-graphene nanocomposite and its application in the magnetic solid phase extraction of sulfonamides from milk samples [J]. Talanta, 2015, 144: 1279−1286. doi: 10.1016/j.talanta.2015.08.006
[28]	FU L, ZHOU H, MIAO E M, et al. Functionalization of amino terminated carbon nanotubes with isocyanates for magnetic solid phase extraction of sulfonamides from milk and their subsequent determination by liquid chromatography-high resolution mass spectrometry [J]. Food Chemistry, 2019, 289: 701−707. doi: 10.1016/j.foodchem.2019.03.097