LC-MS/MS Determination of Residual Amounts of Sulfonamides and Quinolones in Aquatic Products
摘 要
水产品样品(5.00 g)经乙腈-甲酸(99+1)混合液20 mL提取,无水乙醇除水,浓缩并加正己烷2 mL脱脂。所得溶液进行液相色谱分离。以ACQUITY UPLC BEH HILIC色谱柱为分离柱,以不同体积比的甲醇和0.1%(体积分数)甲酸溶液的混合液为流动相进行梯度洗脱。质谱分析中,采用电喷雾正离子源多反应监测模式检测。采用内标法定量。所涉11种药物的线性范围均为5~200 μg·L-1,方法的测定下限(10S/N)在0.07~0.20 μg·kg-1之间。在1.0,4.0,20.0 μg·kg-1等3个浓度水平进行加标回收试验,回收率在80.3%~119%之间,测定值的相对标准偏差(n=6)在1.3%~12%之间。
Abstract
The sample of aquatic products (5.00 g) was extracted with 20 mL of a mixture of acetonitrile and formic acid (99+1). The extract was dehydrated with absolute ethanol. The extract was then concentrated and 2 mL of n-hexane was added to remove fat. LC separation was performed by using ACQUITY UPLC BEH HILIC chromatographic column as stationary phase, and mixtures of methanol and 0.1% (φ) formic acid solution with various ratios as mobile phase in gradient elution. ESI+ and multi-reaction-monitoring were adopted in MS/MS. Internal standard method was used for quantification. Linearity ranges of the 11 drugs were found in the same range of 5-200 μg·L-1, with lower limits of determination (10S/N) in the range of 0.07-0.20 μg·kg-1. Tests for recovery were made by standard addition method at 3 concentration levels of 1.0, 4.0, 20.0 μg·kg-1, giving values of recovery and RSD's (n=6) in the ranges of 80.3%-119% and 1.3%-12% respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201705007
所属栏目 工作简报
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收稿日期 2016/5/11
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备注李婵君(1978-),女,河南新密人,主要从事农产品质量检测工作,chanjunli@163.com
引用该论文: LI Chanjun,LI Zhumei,QIN Xiling,DONG Sujing,WANG Yanchao. LC-MS/MS Determination of Residual Amounts of Sulfonamides and Quinolones in Aquatic Products[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(5): 527~531
李婵君,李柱梅,秦喜玲,董素静,王彦超. 液相色谱-串联质谱法测定水产品中磺胺类及喹诺酮类药物残留量[J]. 理化检验-化学分册, 2017, 53(5): 527~531
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【2】JUHEL-GAUGAIN M, ABJEAN J P. Screening of quinolone resvidues in pig muscle by planar chromatography[J]. Chrornatographia, 1998,47:101-104.
【3】ZENG Z, DONG A, RANG G, et al. Simultaneous determination of nine fluoroquinolones in egg white and egg yolk by liquid chromatography with fluorescence detection[J]. J Chromatogr B, 2005,821(2):202-209.
【4】杜黎明,卫洪清,张俊燕,等.反相高效液相色谱法同时测定6种氟喹诺酮类药物[J].色谱, 2003,5(7):503-506.
【5】胡献刚,罗义,周启星,等.固相萃取-高效液相色谱法测定畜牧粪便中13种抗生素药物残留[J].分析化学, 2008,36(9):1162-1166.
【6】刘亚梅,闵盛.高效液相色谱法同时测定禽蛋中环丙沙星、达氟沙星和恩诺沙星的残留量[J].理化检验-化学分册, 2016,52(3):305-307.
【7】孟勇,张美琴,王静,等.高效液相色谱法测定水产品中7种兽药残留量[J].理化检验-化学分册, 2012,48(5):543-546.
【8】张林田,黄少玉,陈小雪,等.高效液相色谱法测定水产品中四种氟喹诺酮类药物残留[J].理化检验-化学分册, 2009,45(9):1086-1087.
【9】TOUSSAINT B, BORDIN G, JANOSI A, et al. Validation of a liquid chromatography-tandem mass spectrometry method for the smiultaneous quantification of 11(fluoro) quinolone antibiotics in swine kidney[J]. J Chromatogr A, 2002,976(1/2):195-206.
【10】LIM J, PARK B, YUN H. Sensitive liquid chromautographic. mass spectrometry assay for norfloxacin in poultry tissue[J]. J Chromatogr B, 2002,772:185-189.
【11】王立琦,贺利民,曾振灵,等.液相色谱-串联质谱检测兽药残留中的基质效应的研究进展[J].质谱学报, 2011,32(6):321-332.
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