Determination of 7 Antiviral Drugs Residues in Chicken by Automatic Solid Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry
摘 要
采用全自动固相萃取-液相色谱-串联质谱法快速测定鸡肉中金刚烷胺、金刚乙胺、美金刚、阿昔洛韦、吗啉胍、咪喹莫特和奥司他韦等7种抗病毒药物的残留量。样品用体积比为1:1的乙腈-1%(质量分数)三氯乙酸溶液的混合液提取,经全自动固相萃取仪净化,以Hilic Plus亲水色谱柱为固定相,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,采用同位素内标法定量分析。结果表明:7种抗病毒药物的质量浓度均在1.0~20 μg·L-1内与其定量离子与内标的峰面积的比值呈线性关系,检出限(3S/N)为0.03~0.3 μg·kg-1。按标准加入法进行回收试验,回收率为75.7%~105%,测定值的相对标准偏差(n=6)均小于5.0%。与国家标准及行业标准相比,方法在保证高提取率的前提下实现了仪器自动化,且避免了试验人员过多接触有机试剂。
Abstract
Automatic solid phase extraction-liquid chromatography-tandem mass spectrometry (automatic-SPE-LC-MS/MS) was applied to rapid determination of the 7 antiviral drugs (induding amantadine, rimantadine, memantine, acyclovir, moroxydine, imiquimod and oseltamivir) residues in chicken. The sample was extracted with a mixture of acetonitrile-1% (mass fraction) trichloroacetic acid solution at volume ratio of 1:1, and purified by automatic-SPE system. The chromatographic separation was performed by using Hilic Plus hydrophilic chromatographic column as stationary phase, and the mixtures of methanol and 0.1% (φ) formic acid solution at different volume ratios as mobile phase for gradient elution. Isotope internal standard method was used for quantitative analysis. It was showed that linear relationships between peak area ratio of quantitative ion to internal standard and mass concentration of the 7 antiviral drugs were found in the same range of 1.0-20 μg·L-1, with detection limits (3S/N) in the range of 0.03-0.3 μg·kg-1. Test for recovery was made by standard addition method, giving results in the range of 75.7%-105%, and RSDs (n=6) of the determined values were less than 5.0%. Compared with national standard and industry standard, this method achieved automation of instrument on the premise of high extraction efficiency, and protected the experimental personnel from being exposed to organic reagents.
中图分类号 O652.53 DOI 10.11973/lhjy-hx202112004
所属栏目 工作简报
基金项目 浙江省科技厅公益项目(LGF21B050001)
收稿日期 2020/5/4
修改稿日期
网络出版日期
作者单位点击查看
备注傅红雪,工程师,硕士,研究方向为食品安全与分析技术
引用该论文: FU Hongxue,CHEN Wanqin,CHEN Bilian,LIU Zhu,LIANG Jingjing,WANG Feng. Determination of 7 Antiviral Drugs Residues in Chicken by Automatic Solid Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(12): 1082~1088
傅红雪,陈万勤,陈碧莲,刘柱,梁晶晶,王峰. 全自动固相萃取-液相色谱-串联质谱法测定鸡肉中7种抗病毒药物残留量[J]. 理化检验-化学分册, 2021, 57(12): 1082~1088
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】艾连峰,马育松,陈瑞春,等.在线净化液相色谱-串联质谱法测定动物源食品中金刚烷胺的残留[J].分析化学, 2013,41(8):1194-1198.
【2】易锡斌,裘立群,刘世琦,等.液相色谱-串联质谱同时测定禽肉组织中盐酸金刚烷胺、盐酸金刚乙胺、地塞米松、替米考星及喹乙醇代谢物的残留量[J].分析测试学报, 2015,34(3):346-351.
【3】DONG G, PENG C, LUO J, et al. Adamantane-resistant influenza a viruses in the world (1902-2013):Frequency and distribution of M2 gene mutations[J]. PLoS One, 2015,10(3):e0119115.
【4】DURRANT M G, EGGETT D L, BUSATH D D. Investigation of a recent rise of dual amantadine-resistance mutations in the influenza A M2 sequence[J]. BMC Genetics, 2015,16(2):1-9.
【5】WILLS R J, FAROLINO D A, CHOMA N, et al. Rimantadine pharmacokinetics after single and multiple doses[J]. Antimicrobial Agents and Chemotherapy, 1987,31(5):826-828.
【6】TOMINACK R L, WILLS R J, GUSTAVSON L E, et al. Multiple-dose pharmacokinetics of rimantadine in elderly adults[J]. Antimicrob Agents Chemother, 1988,32(12):1813-1819.
【7】LABORDE-KUMMER E, GAUDIN K, JOSEPH-CHARLES J, et al. Development and validation of a rapid capillary electrophoresis method for the determination of oseltamivir phosphate in Tamiflu® and generic versions[J]. Journal of Pharmaceutical and Biomedical Analysis, 2009,50(3):544-546.
【8】王夏炎,钱木水.气相色谱法测定盐酸金刚乙胺口服液的含量[J].中国现代应用药学, 2004(5):392-394.
【9】DOU Y, SUN Y, REN Y Q, et al. Simultaneous non-destructive determination of two components of combined paracetamol and amantadine hydrochloride in tablets and powder by NIR spectroscopy and artificial neural networks[J]. Journal of Pharmaceutical and Biomedical Analysis, 2005,37(3):543-549.
【10】JALALI F, MAGHOOLI R. Potentiometric determination of trace amounts of amantadine using a modified carbon-paste electrode[J]. Analytical Sciences, 2009,25(10):1227-1230.
【11】FARAJZADEH M A, NOURI N, ALIZADEH NABIL A A. Determination of amantadine in biological fluids using simultaneous derivatization and dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection[J]. Journal of Chromatography B, 2013,940:142-149.
【12】HEROLD D A, ANONICK P K, KINTER M, et al. Measurement of rimantadine in plasma by capillary gas chromatography/mass spectrometry with a deuterium-labeled internal standard[J]. Clinical Chemistry, 1988,34(8):1597-1599.
【13】JING S J, LI Q L, JIANG Y. A new simultaneous derivatization and microextration method for the determination of memantine hydrochloride in human plasma[J]. Journal of Chromatography B, 2016,1008:26-31.
【14】CHAN D, TARBIN J, SHARMAN M, et al. Screening method for the analysis of antiviral drugs in poultry tissues using zwitterionic hydrophilic interaction liquid chromatography/tandem mass spectrometry[J]. Analytica Chimica Acta, 2011,700(1/2):194-200.
【15】庾金良,张晓燕,卜洪忠,等.高效液相色谱-串联质谱法测定鸡肉产品中金刚烷胺残留量[J].理化检验-化学分册, 2015,51(2):224-227.
【16】中华人民共和国国家质量监督检验检疫总局.出口动物组织中抗病毒类药物残留量的测定液相色谱-质谱/质谱法:SN/T 4253-2015[S].北京:中国标准出版社, 2016.
【17】中华人民共和国农业农村部,国家卫生健康委员会,国家市场监督管理总局.食品安全国家标准动物性食品中金刚烷胺残留量的测定液相色谱-串联质谱法:GB 31660.5-2019[S].北京:中国标准出版社, 2019.
【2】易锡斌,裘立群,刘世琦,等.液相色谱-串联质谱同时测定禽肉组织中盐酸金刚烷胺、盐酸金刚乙胺、地塞米松、替米考星及喹乙醇代谢物的残留量[J].分析测试学报, 2015,34(3):346-351.
【3】DONG G, PENG C, LUO J, et al. Adamantane-resistant influenza a viruses in the world (1902-2013):Frequency and distribution of M2 gene mutations[J]. PLoS One, 2015,10(3):e0119115.
【4】DURRANT M G, EGGETT D L, BUSATH D D. Investigation of a recent rise of dual amantadine-resistance mutations in the influenza A M2 sequence[J]. BMC Genetics, 2015,16(2):1-9.
【5】WILLS R J, FAROLINO D A, CHOMA N, et al. Rimantadine pharmacokinetics after single and multiple doses[J]. Antimicrobial Agents and Chemotherapy, 1987,31(5):826-828.
【6】TOMINACK R L, WILLS R J, GUSTAVSON L E, et al. Multiple-dose pharmacokinetics of rimantadine in elderly adults[J]. Antimicrob Agents Chemother, 1988,32(12):1813-1819.
【7】LABORDE-KUMMER E, GAUDIN K, JOSEPH-CHARLES J, et al. Development and validation of a rapid capillary electrophoresis method for the determination of oseltamivir phosphate in Tamiflu® and generic versions[J]. Journal of Pharmaceutical and Biomedical Analysis, 2009,50(3):544-546.
【8】王夏炎,钱木水.气相色谱法测定盐酸金刚乙胺口服液的含量[J].中国现代应用药学, 2004(5):392-394.
【9】DOU Y, SUN Y, REN Y Q, et al. Simultaneous non-destructive determination of two components of combined paracetamol and amantadine hydrochloride in tablets and powder by NIR spectroscopy and artificial neural networks[J]. Journal of Pharmaceutical and Biomedical Analysis, 2005,37(3):543-549.
【10】JALALI F, MAGHOOLI R. Potentiometric determination of trace amounts of amantadine using a modified carbon-paste electrode[J]. Analytical Sciences, 2009,25(10):1227-1230.
【11】FARAJZADEH M A, NOURI N, ALIZADEH NABIL A A. Determination of amantadine in biological fluids using simultaneous derivatization and dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection[J]. Journal of Chromatography B, 2013,940:142-149.
【12】HEROLD D A, ANONICK P K, KINTER M, et al. Measurement of rimantadine in plasma by capillary gas chromatography/mass spectrometry with a deuterium-labeled internal standard[J]. Clinical Chemistry, 1988,34(8):1597-1599.
【13】JING S J, LI Q L, JIANG Y. A new simultaneous derivatization and microextration method for the determination of memantine hydrochloride in human plasma[J]. Journal of Chromatography B, 2016,1008:26-31.
【14】CHAN D, TARBIN J, SHARMAN M, et al. Screening method for the analysis of antiviral drugs in poultry tissues using zwitterionic hydrophilic interaction liquid chromatography/tandem mass spectrometry[J]. Analytica Chimica Acta, 2011,700(1/2):194-200.
【15】庾金良,张晓燕,卜洪忠,等.高效液相色谱-串联质谱法测定鸡肉产品中金刚烷胺残留量[J].理化检验-化学分册, 2015,51(2):224-227.
【16】中华人民共和国国家质量监督检验检疫总局.出口动物组织中抗病毒类药物残留量的测定液相色谱-质谱/质谱法:SN/T 4253-2015[S].北京:中国标准出版社, 2016.
【17】中华人民共和国农业农村部,国家卫生健康委员会,国家市场监督管理总局.食品安全国家标准动物性食品中金刚烷胺残留量的测定液相色谱-串联质谱法:GB 31660.5-2019[S].北京:中国标准出版社, 2019.
相关信息