UHPLC-MS/MS Determination of Dexamethasone Betamethasone and Beclomethasone in Pork
摘 要
提出了猪肉中糖皮质激素类药物地塞米松、倍他米松、倍氯米松同时测定的超高效液相色谱-串联质谱法(UHPLC-MS/MS),采用串联四极杆质谱仪及超高效液相色谱仪联用.质谱离子源为电喷雾电离,检测方式为多反应监测正离子模式.超高压反相C18色谱柱分离,以不同比例配成的甲酸-水(1+999)溶液及乙腈的混合溶液作流动相进行梯度洗脱.上述3种药物的质量浓度在1.0~100.0 μg·L-1范围内呈线性.方法的回收率在83%~96%之间,地塞米松、倍他米松和倍氯米松的测定下限(10S/N)分别为1,1,2 μg·kg-1.
Abstract
A method of determination of residual amounts of dexamethasone,betamethasone and beclomethasone in pork by hyphenation of UHPLC with MS/MS (in tandem) was proposed.The temdem quadripole mass spectrometer in hyphenation with ultra high performance liquid chromatography with ionization source of ESI+ and detection mode of MRM was used in the analysis.The C18 column was used as stationary phase,and mixtures of dil.formic acid (1+999) and acetonitrile in different proportions were used as mobile phase in the gradient elution of chromatographic separation.Linear relationships between values of analytical signal and mass concentration of the 3 drugs were obtained in the range from 1.0 to 100.0 μg·L-1.Results of recovery test were found in the range from 83% to 96%,and values of lower limit of determination (10S/N) found were 1 μg·kg-1 for dexamethasone and betamethasone,and 2 μg·kg-1 for beclomethasone.
中图分类号 O652.63
所属栏目 工作简报
基金项目 国家质量监督检验检疫总局科研计划资助项目(2007IK137)
收稿日期 2009/5/1
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备注吴敏(1974-),女,福建人,高级工程师,研究方向食品有毒有害物质残留分析.
引用该论文: WU Min,ZHENG Xiang-hua,QI Shi-lin,HONG Yu-chen,ZHOU Yu. UHPLC-MS/MS Determination of Dexamethasone Betamethasone and Beclomethasone in Pork[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(11): 1282~1285
吴敏,郑向华,齐士林,洪煜琛,周昱. 超高效液相色谱-串联质谱测定猪肉中地塞米松、倍他米松和倍氯米松[J]. 理化检验-化学分册, 2010, 46(11): 1282~1285
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参考文献
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【2】ZHAO Shan,WU Da-nan,WANG Peng.Simultaneous determination of seven sexual hormonesin cosmetics by reversed-phase high performance liquid chromatography[J].J Chin J Chromatogr,2004,22(3):267-269.
【3】SHEARAN P,O′KEEFFE M,SMYTH M R.Reversed-phase high-performance liquid chromatographic determination of dexamethasone in bovine tissue[J].J Analyst,1991,116:1365-1368.
【4】IGLESIAS Y,FENTE C A,VZQUEZ B,et al.Determination of dexamethasone in bovine liver by chemiluminescence high-performance liquid chromatography[J].J Agric Food Chem,1999,47:4275-4279.
【5】MALLINSON E TH,DREAS J S,WILSON R T,et al.Determination of dexamethasone in liver and muscle by liquid chromatography and gas chromatography/mass spectrometry[J].J Agri Food Chem,1995,43:140-145.
【6】HARRISON L I,KURUP S,WAGNER C,et al.Pharmacokinetics of beclomethasone 17-monopropionate from a beclomethasone dipropionate extra fine aerosol in adults with asthma[J].J Eur J Clin Pharmacol,2002,58(3):197-201.
【7】TAYLOR R L,GREBE S K,QUANTITATIVE R J S.Highly sensitive liquid chromatography-tandem mass spectrometry method for detection of synthetic corticosteroids[J].J Clinical Chemistry,2004,50(12):2345-2352.
【8】ANTIGNAC J P.Multi-residue extraction-purification procedure for corticosteroids in biological samples for efficient control of their misuse in livestock production[J].Journal of Chromatography B,2001,757: 11-19.
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