Simultaneous Determination of 10 Kinds of Aminoglycosides in Aquatic Products by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
-
摘要: 【目的】建立同时检测水产品中壮观霉素、潮霉素B、双氢链霉素、链霉素、丁胺卡那霉素、卡那霉素、安普霉素、妥布霉素、庆大霉素、新霉素等10种氨基糖苷类药物的超高效液相色谱-串联质谱（UPLC-MS/MS）方法。【方法】样品用10 mmol/L磷酸二氢钾缓冲溶液提取，用氢氧化钠溶液将提取液的pH调为6.6~7.0，取一半体积提取液上HLB固相萃取柱净化，采用Obelisc R柱高效分离，电喷雾正离子多反应监测模式监测。【结果与结论】10种氨基糖苷类药物呈现良好的线性关系（R2> 0.999），新霉素的检出限和定量限分别为5.0、10.0 μg/kg，潮霉素B和安普霉素的检出限和定量限分别为2.0、5.0 μg/kg，其余7种氨基糖苷类药物的检出限和定量限分别为1.0 μg/kg和2.0 μg/kg。10种分析物的加标回收率为74.8%~104.5%，相对标准偏差（RSD）为4.5%~12.6%。本方法分析时间短，5 min内即完成10种药物的分离，分析物峰形尖锐。方法灵敏度、准确度高，适用于水产品中10种氨基糖苷类药物的同时测定。
-
关键词:
- 水产品 /
- 氨基糖苷类药物 /
- 药物残留检测 /
- 超高效液相色谱-串联质谱
Abstract: 【Objective】An ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous determination of 10 kinds of aminoglycosides (AGs), including spectinomycin, hygromycin B, dihydrostrepmycin, streptomycin, amikacin, kanamycin, apramycin, tobramycin, gentamycin and neomycin in edible parts of aquatic products. 【Method】The samples were extracted with 10 mmol/L potassium dihydrogen phosphate buffer solution, then the pH of the extract was adjusted to be neutral by sodium hydroxide. Half of the volume was cleaned-up and pre-concentrated using Hydrophile Lipophilic Balance (HLB) cartridge. All the target compounds were separated on an Obelisc R column and detected by UPLC-MS/MS under ESI + ionization Multiple response monitoring (MRM) mode. 【Result and Conclusion】 Under optimized conditions, this method had a good linearity (R2>0.999). The limit of detection (LOD, S/N≥ 3) and the limits of quantification (LOQ, S/N≥10) of neomycin were 5.0 μg/kg and 10.0 μg/kg, respectively; LOD and LOQ of hygromycin B and apramycin were 2.0 μg/kg and 5.0 μg/kg, respectively; LOD and LOQ of the other 7 kinds AGs were 1.0 μg/kg and 2.0 μg/kg, respectively. Besides, the average recoveries presented 78.4%-104.5% with the relative standard deviations (RSDs, n = 6) of 4.5%-12.6%. The analysis was rapid and can be achieved in less than 5 min. The method had the characteristics of high accuracy and good precision, was suitable for simultaneous determination of 10 kinds of AGs in aquatic products. -
-
FOSTER J II, TEKIN M. Aminoglycoside induced ototoxicity associated with mitochondrial DNA mutations[J]. Egyptian Journal of Medical Human Genetics, 2016, 17(3):287-293.
FAROUK F, AZZAZY H M E, NIESSEN W M A. Challenges in the determination of aminoglycoside antibiotics, a review[J]. Analytica Chimica Acta, 2015, 890:21-43.
CAI Y Q, CAI Y E, CHENG J, et al. Comparative study on the analytical performance of three waveforms for the determination of several aminoglycoside antibiotics with high performance liquid chromatography using amperometric detection[J]. Journal of Chromatography A, 2005, 1085(1):124-130.
European Commission. Commission regulation (EU) No. 37/2010 of 22 December 2009:on pharmacologically active substances and their classification regarding maximum residue limits in food stuffs of animal origin[R]. Official Journal of the European Union, 2010:1-72.
LOSOYA-LEAL A, ESTEVEZ M C, MARTÍNEZ-CHAPA S O, et al. Design of a surface plasmon resonance immunoassay for therapeutic drug monitoring of amikacin[J]. Talanta, 2015, 141:253-258.
WANG S, XU B, ZHANG Y, et al. Development of enzyme-linked immunosorbent assay (ELISA) for the detection of neomycin residues in pig muscle, chicken muscle, egg, fish, milk and kidney[J]. Meat Science, 2009, 82(1):53-58.
YANG B X, WANG L, LUO C Y, et al. Simultaneous determination of 11 aminoglycoside residues in honey, milk, and pork by liquid chromatography with tandem mass spectrometry and molecularly imprinted polymer solid phase extraction[J]. Journal of AOAC International, 2017, 100(6):1869-1878.
JIANG Y, HE M Y, ZHANG W J, et al. Recent advances of capillary electrophoresis-mass spectrometry instrumentation and methodology[J]. Chinese Chemical Letters, 2017, 28(8):1640-1652.
MUKHTAR N H, MAMAT N A, SEE H H. Monitoring of tobramycin in human plasma via mixed matrix membrane extraction prior to capillary electrophoresis with contactless conductivity detection[J]. Journal of Pharmaceutical and Biomedical Analysis, 2018, 158:184-188.
PAUL P, SÄNGER-VAN DE GRIEND C, ADAMS E, et al. Recent advances in the capillary electrophoresis analysis of antibiotics with capacitively coupled contactless conductivity detection[J]. Journal of Pharmaceutical and Biomedical Analysis, 2018, 158:405-415.
YU Y, LIU Y, WANG W T, et al. Highly sensitive determination of aminoglycoside residues in food by sheathless CE-ESI-MS/MS[J]. Analytical Methods, 2019, 11(39):5064-5069.
ZHANG L, PENG J D, TANG J X, et al. Description and validation of coupling high performance liquid chromatography with resonance Rayleigh scattering in aminoglycosides determination[J]. Analytica Chimica Acta, 2011, 706(2):199-204.
IANNI F, PUCCIARINI L, CAROTTI A, et al. Hydrophilic interaction liquid chromatography of aminoglycoside antibiotics with a diol-type stationary phase[J]. Analytica Chimica Acta, 2018, 1044:174-180.
KAUFMANN A, BUTCHER P, MADEN K. Determination of aminoglycoside residues by liquid chromatography and tandem mass spectrometry in a variety of matrices[J]. Analytica Chimica Acta, 2012, 711:46-53.
YOUNG M S, VAN TRAN K, GOH E, et al. A rapid SPEbased analytical method for UPLC/MS/MS determination of aminoglycoside antibiotic residues in bovine milk, muscle, and kidney[J]. Journal of AOAC International, 2014, 97(6):1737-1741.
ARSAND J B, JANK L, MARTINS M T, et al. Determination of aminoglycoside residues in milk and muscle based on a simple and fast extraction procedure followed by liquid chromatography coupled to tandem mass spectrometry and time of flight mass spectrometry[J]. Talanta, 2016, 154:38-45.
MORENO-GONZÁLEZ D, HAMED A M, GARCÍACAMPAÑA A M, et al. Evaluation of hydrophilic interaction liquid chromatography-tandem mass spectrometry and extraction with molecularly imprinted polymers for determination of aminoglycosides in milk and milk-based functional foods[J]. Talanta, 2017, 171:74-80.
KIM Y R, KANG H S. Multi-residue determination of twenty aminoglycoside antibiotics in various food matrices by dispersive solid phase extraction and liquid chromatography-tandem mass spectrometry[J]. Food Control, 2021, 130:108374.
WANG Y, LI S H, ZHANG F F, et al. Study of matrix effects for liquid chromatography-electrospray ionization tandem mass spectrometric analysis of 4 aminoglycosides residues in milk[J]. Journal of Chromatography A, 2016, 1437:8-14.
FENG J N, SHE X J, HE X Y, et al. Synthesis of magnetic graphene/mesoporous silica composites with boronic acidfunctionalized pore-walls for selective and efficient residue analysis of aminoglycosides in milk[J]. Food Chemistry, 2018, 239:612-621.
YUE F L, LI H, KONG Q Q, et al. Selection of broadspectrum aptamer and its application in fabrication of aptasensor for detection of aminoglycoside antibiotics residues in milk[J]. Sensors and Actuators B:Chemical, 2022, 351:130959.
WU Q, ABU BAKR SHABBIR M, PENG D P, et al. Microbiological inhibition-based method for screening and identifying of antibiotic residues in milk, chicken egg and honey[J]. Food Chemistry, 2021, 363:130074.
TAO Y F, CHEN D M, YU H, et al. Simultaneous determination of 15 aminoglycoside (s) residues in animal derived foods by automated solid-phase extraction and liquid chromatography-tandem mass spectrometry[J]. Food Chemistry, 2012, 135(2):676-683.
SALUTI G, DIAMANTI I, GIUSEPPONI D, et al. Simultaneous determination of aminoglycosides and colistins in food[J]. Food Chemistry, 2018, 266:9-16.
LI D, LI T F, WANG L, et al. A polyvinyl alcohol-coated core-shell magnetic nanoparticle for the extraction of aminoglycoside antibiotics residues from honey samples[J]. Journal of Chromatography A, 2018, 1581/1582:1-7.
WANG X R, YANG S P, LI Y, et al. Optimization and application of parallel solid-phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry for the determination of 11 aminoglycoside residues in honey and royal jelly[J]. Journal of Chromatography A, 2018, 1542:28-36.
WU D, LIU P, FAN W J, et al. Design of green coating material of combining rigid and flexible properties for the extraction of aminoglycosides residues[J]. Journal of Chromatography A, 2021, 1641:462006.
GLINKA M, WOJNOWSKI W, WASIK A. Determination of aminoglycoside antibiotics:current status and future trends[J]. Trends in Analytical Chemistry, 2020, 131:116034.
JANDERA P. Stationary and mobile phases in hydrophilic interaction chromatography:a review[J]. Analytica Chimica Acta, 2011, 692(1/2):1-25.
ZHOU G S, PANG H Q, TANG Y P, et al. Hydrophilic interaction ultra-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (HILIC-UPLC-TQ-MS/MS) in multiple-reaction monitoring (MRM) for the determination of nucleobases and nucleosides in ginkgo seeds[J]. Food Chemistry, 2014, 150:260-266.
HUA W Y, IERARDI T, LESSLIE M, et al. Development and validation of a HILIC-MS/MS method for quantification of decitabine in human plasma by using lithium adduct detection[J]. Journal of Chromatography B, 2014, 969:117-122.
KUMAR P, RUBIES A, COMPANYÓ R, et al. Hydrophilic interaction chromatography for the analysis of aminoglycosides[J]. Journal of Separation Science, 2012, 35(4):498-504.
计量
- 文章访问数: 797
- PDF下载数: 1
- 施引文献: 0
下载:
