QuEChERS-高效液相色谱-串联质谱法同时测定有机肥料中10种氟喹诺酮类药物残留
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摘要
分析检测有机肥料中的兽药残留对于评价土壤微生物群落和人类健康的潜在风险至关重要。该文建立了一种QuEChERS联用高效液相色谱-串联质谱(HPLC-MS/MS)同时检测有机肥料中10种氟喹诺酮类药物残留的分析方法。样品经乙二胺四乙酸二钠(Na_2EDTA)-Mcllvaine缓冲溶液(pH=4.0)和乙腈提取,采用Atlantis T3 C_(18)色谱柱(250 mm×4.6 mm, 5μm),以0.2%(体积分数)甲酸水溶液和乙腈为梯度洗脱的流动相,采用电喷雾离子(ESI)源,在多反应监测(MRM)扫描模式下进行检测。10种氟喹诺酮类药物用内标法定量。结果表明,10种氟喹诺酮类药物在10～500μg/kg范围内线性关系良好,相关系数均大于0.993 0。方法检出限为0.5～2.5μg/kg,定量限为1.7～8.3μg/kg。该分析方法成功应用于9个有机肥样品的兽药污染调查。结果显示,样品的平均加标回收率为82.5%～117.1%,相对标准偏差为3.4%～10.2%。该方法准确可靠、灵敏度高,能够满足多种兽药残留的同时检测,该方法有望为有机肥料兽药风险评估提供依据。
The analysis of veterinary drugs in organic fertilizers is crucial for an assessment of their potential risks to microbial communities in soils and to human health. A method has been developed for the simultaneous determination of ten fluoroquinolones in organic fertilizers by using the QuEChERS method coupled with high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). The sample was extracted with disodium ethylenediaminetetraacetic acid(Na_2EDTA)-McIlvaine buffer(pH=4.0) and acetonitrile. The target compounds were separated on an Atlantis T3 C18 column(250 mm×4.6 mm, 5 μm) with a mobile phase of 0.2%(v/v) formic acid in acetonitrile and analyzed in the multiple reaction monitoring(MRM) mode via electrospray ionization(ESI). Ten fluoroquinolones were quantified by an internal standard method. The calibration curves of the ten fluoroquinolones exhibited good linearity over the range of 10-500 μg/kg, and the correlation coefficients were above 0.993 0. The limits of detection were 0.5-2.5 μg/kg; the limits of quantification were 1.7-8.3 μg/kg. The analytical method was successfully applied in a survey of veterinary drug contamination in nine compost samples. The average recoveries were 82.5%-117.1%, with relative standard deviations of 3.4%-10.2%. The method is accurate, reliable, and sensitive and supports the simultaneous detection of various veterinary drug residues. Therefore, this method can provide a basis for the risk assessment of veterinary drugs in organic fertilizers.
The analysis of veterinary drugs in organic fertilizers is crucial for an assessment of their potential risks to microbial communities in soils and to human health. A method has been developed for the simultaneous determination of ten fluoroquinolones in organic fertilizers by using the QuEChERS method coupled with high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). The sample was extracted with disodium ethylenediaminetetraacetic acid(Na_2EDTA)-McIlvaine buffer(pH=4.0) and acetonitrile. The target compounds were separated on an Atlantis T3 C18 column(250 mm×4.6 mm, 5 μm) with a mobile phase of 0.2%(v/v) formic acid in acetonitrile and analyzed in the multiple reaction monitoring(MRM) mode via electrospray ionization(ESI). Ten fluoroquinolones were quantified by an internal standard method. The calibration curves of the ten fluoroquinolones exhibited good linearity over the range of 10-500 μg/kg, and the correlation coefficients were above 0.993 0. The limits of detection were 0.5-2.5 μg/kg; the limits of quantification were 1.7-8.3 μg/kg. The analytical method was successfully applied in a survey of veterinary drug contamination in nine compost samples. The average recoveries were 82.5%-117.1%, with relative standard deviations of 3.4%-10.2%. The method is accurate, reliable, and sensitive and supports the simultaneous detection of various veterinary drug residues. Therefore, this method can provide a basis for the risk assessment of veterinary drugs in organic fertilizers.
引文
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[4] Li W H, Shi Y L, Gao L H, et al. Journal of Instrumental Analysis, 2010, 29(10): 987 厉文辉, 史亚利, 高立红, 等. 分析测试学报, 2010, 29(10): 987
[5] He D C. [PhD Dissertation]. Changsha: Hunan Agricultural University, 2011 贺德春. [博士学位论文]. 长沙: 湖南农业大学, 2011
[6] Zhang J Q, Dong Y H, An Q, et al. Soils, 2005, 37(4): 353 张劲强, 董元华, 安琼, 等. 土壤, 2005, 37(4): 353
[7] Zhang J H, Meng T, Zhou Z H, et al. China Animal Husbandry and Veterinary Medicine, 2014, 41(5): 262 张家禾, 孟婷, 周作红, 等. 中国畜牧兽医, 2014, 41(5): 262
[8] Li X P, Jiang J Q, Qian A D, et al. Progress in Veterinary Medicine, 2013, 34(9): 99 李新朋, 姜金庆, 钱爱东, 等. 动物医学进展, 2013, 34(9): 99
[9] Qian Z Z, Liang Y, Wang L J, et al. Fisheries Research, 2018, 40(4): 286 钱卓真, 梁焱, 王丽娟, 等. 渔业研究, 2018, 40(4): 286
[10] Qiu P Z, Guo X Y, Wang N, et al. Chinese Journal of Chromatography, 2015, 33(7): 722 邱盼子, 郭欣妍, 王娜, 等. 色谱, 2015, 33(7): 722
[11] Yang Y F, Cao X M, Li X L, et al. Chinese Journal of Chromatography, 2016, 34(11): 1063 杨艳菲, 曹旭敏, 李雪莲, 等. 色谱, 2016, 34(11): 1063
[12] Li L, Liu F, Chen H H, et al. Chinese Journal of Chromatography, 2013, 31(6): 567 李璐, 刘菲, 陈鸿汉, 等. 色谱, 2013, 31(6): 567
[13] Tong Y K, Hu Y, Xia Q F, et al. Chinese Journal of Chromatography, 2017, 35(3): 291 佟育奎, 胡月, 夏琴飞, 等. 色谱, 2017, 35(3): 291
[14] Jacobsen A M, Halling-S?rensen B. Anal Bioanal Chem, 2006, 384: 1164
[15] Ho Y B, Zakaria M P, Latif P A, et al. J Chromatogr A, 2012, 1262: 160
[16] Chen Y, Zhang H, Luo Y, et al. Chinese Sci Bull, 2012, 57: 606
[17] DorivalGarcí N, LabajoRecio C, Zafra-Gómez A, et al. Talanta, 2015, 138: 247
[18] Speltini A, Sturini M, Maraschi F, et al. J Chromatogr A, 2015, 1410: 44
[19] Yang J Y, Zhang Y, Zeng D P, et al. Science and Technology of Food Industry, 2015(1): 292 杨金易, 张燕, 曾道平, 等. 食品工业科技, 2015(1): 292
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