超高效液相色谱-四极杆飞行时间质谱法测定克氏螯虾中39种兽药残留
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摘要
建立了超高效液相色谱-四极杆飞行时间质谱(UHPLC-Q-TOF-MS)快速筛查克氏螯虾中39种兽药残留的分析方法。样品经酸化乙腈提取,增强型脂质去除净化剂(EMR-Lipid)结合石墨化多壁碳纳米管(GMWNTs)净化,采用UHPLC-Q-TOF-MS分析检测。通过比对待测物准分子离子的精确质量数、同位素丰度比、保留时间等特征信息进行定性初筛,通过二级谱图谱库检索比对进行确证,通过一级提取离子色谱图峰面积进行定量分析。39种化合物在各自的浓度范围内均呈良好的线性关系,线性相关系数均大于0.99,定量限为3～15μg/kg,添加回收率为62. 4%～105. 8%,相对标准偏差(RSD)为2. 5%～13. 5%,方法简便、快速、准确,可应用于克氏螯虾中喹诺酮类、磺胺类、三苯甲烷类39种药物残留的快速筛查定量。
An ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UHPLC-Q-TOF-MS)method was developed for determination of 39 veterinary drugs in Procambarusclarkii. Samples were extracted with acidified acetonitrile and purified with enhanced matrix removal-lipid(EMR-Lipid)adsorbent and graphitized multi-walled carbon nanotubes(GMWNTs). Extracts were analyzed by UHPLC-Q-TOF-MS. Target compounds were screened according to accurate mass,isotopic ratio,and retention time,and confirmed by library search. Target analytes were quantified using the chromatographic peak area of each compound. For each of the drugs of interest,calibration curves were linear in their respective ranges with correlation coefficients greater than 0. 99. The limits of quantification(LOQs)were3-15 μg/kg. The recoveries for target compounds spiked in Procambarusclarkii ranged from62. 4% to 105. 8%,with relative standard deviations(RSDs)ranging from 2. 5% to 13. 5%. This method is simple,rapid,accurate,and suitable for simultaneous determination of 39 veterinary drugs,including sulfonamides,quinolones,and triphenylmethane,extracted from Procambarusclarkii.
An ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UHPLC-Q-TOF-MS)method was developed for determination of 39 veterinary drugs in Procambarusclarkii. Samples were extracted with acidified acetonitrile and purified with enhanced matrix removal-lipid(EMR-Lipid)adsorbent and graphitized multi-walled carbon nanotubes(GMWNTs). Extracts were analyzed by UHPLC-Q-TOF-MS. Target compounds were screened according to accurate mass,isotopic ratio,and retention time,and confirmed by library search. Target analytes were quantified using the chromatographic peak area of each compound. For each of the drugs of interest,calibration curves were linear in their respective ranges with correlation coefficients greater than 0. 99. The limits of quantification(LOQs)were3-15 μg/kg. The recoveries for target compounds spiked in Procambarusclarkii ranged from62. 4% to 105. 8%,with relative standard deviations(RSDs)ranging from 2. 5% to 13. 5%. This method is simple,rapid,accurate,and suitable for simultaneous determination of 39 veterinary drugs,including sulfonamides,quinolones,and triphenylmethane,extracted from Procambarusclarkii.
引文
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[5] Chen Z G,Zhan C R,Guo P,et al. Food Science,2007,28(10):448陈振桂,占春瑞,郭平,等.食品科学,2007,28(10):448
[6] Wang C Y,Wang Y P,Wang N,et al. Chinese Journal of Analytical Chemistry,2013,41(1):83王重洋,王远鹏,王宁,等.分析化学,2013,41(1):83
[7] Huang D M,Huang X Y,Gu R R,et al. Chinese Journal of Chromatography,2014,32(8):874黄冬梅,黄宣运,顾润润,等.色谱,2014,32(8):874
[8] Li H,Kijak P J,Turnipseed S B,et al. J Chromatogr B,2006,836(1/2):22
[9] Li N,Zhang Y T,Liu L,et al. Chinese Journal of Chromatography,2014,32(12):1313李娜,张玉婷,刘磊,等.色谱,2014,32(12):1313
[10] Kung T A,Tsai C W,Ku B C,et al. Food Chem,2015,175:189
[11] Zhang Z W,Li X W,Ding S Y,et al. Food Chem,2016,204:252
[12] Chen Y S,Schwack W. J Chromatogr A,2013,1312:143
[13] Li X J,Peng T,Li C J. Journal of Instrumental Analysis,2012,31(5):628李晓娟,彭涛,李重九.分析测试学报,2012,31(5):628
[14] Meng Z,Shi Z H,LüY K,et al. Chinese Journal of Analytical Chemistry,2014,42(10):1493孟哲,石志红,吕运开,等.分析化学,2014,42(10):1493
[15] Huang L,Dai Y F,Wang P Y,et al. Chinese Journal of Chromatography,2015,33(10):1097黄鹂,戴意飞,王萍亚,等.色谱,2015,33(10):1097
[16] Kaufmann A,Butcher P,Maden K,et al. J Chromatogr A,2008,1194(1):66
[17] Li N,Zhang Y T,Liu L,et al. Chinese Journal of Chromatography,2014,32(12):1313李娜,张玉婷,刘磊,等.色谱,2014,32(12):1313
[18] Zhang K M,Liang F Y,Deng M,et al. Chinese Journal of Chromatography,2016,34(9):860张科明,梁飞燕,邓鸣,等.色谱,2016,34(9):860
[19] Wang F,Mi J B,Li S J,et al. Journal of Instrumental Analysis,2017,36(2):272王飞,宓捷波,李淑静,等.分析测试学报,2017,36(2):272
[20] Zhang F Y,Jiang W F,Wang X Q. China Dairy Industry,2018(4):57张凤艳,蒋万枫,王锡青.中国乳品工业,2018(4):57
[21] Lu Y,Cheng Z,Liu C,et al. Food Anal Methods,2016,9(6):1857
[22] Li J,Zhang J,Liu H,et al. J Sci Food Agr,2016,96(2):555
[23] Peng X J,Zeng L Z,Wu C C,et al. Journal of Instrumental Analysis,2017,36(6):738彭晓俊,曾丽珠,伍长春,等.分析测试学报,2017,36(6):738
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[25] GB/T 19857-2005
[26] GB/T 20366-2006