| 超高效液相色谱-串联质谱法测定鸡肉和鸡蛋中5种硝基咪唑类药物残留量 |
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| 引用本文： | 凌莉,曲良娇,梁素丹,张艳.超高效液相色谱-串联质谱法测定鸡肉和鸡蛋中5种硝基咪唑类药物残留量[J].现代预防医学,2022,0(16):3029-3035. |
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| 作者姓名： | 凌莉 曲良娇 梁素丹 张艳 |
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| 作者单位： | 珠海市疾病预防控制中心理化检验所，广东 珠海 519060 |
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| 摘 要： | 目的 采用超高效液相色谱-串联质谱法（UPLC-MS/MS），建立鸡肉和鸡蛋中5种硝基咪唑类药物的检测方法。方法 样品经乙腈提取后，加入无水Na2SO4和NaCl，离心后上清液通过PRiME HLB固相萃取小柱净化，滤出液和乙腈洗脱液经氮吹至近干，10%甲醇水（v/v）溶液定容。以0.1 %甲酸水-甲醇为流动相，被测物经BEH C18柱(2.1 mm × 100 mm，1.7 μm)分离、正离子多反应监测模式检测，内标法定量。结果 5种硝基咪唑在0.2～20.0 ng/ml范围内相关系数均大于0.999，方法检出限为0.05～0.10 μg/kg，定量限为0.15～0.30 μg/kg。在3个加标水平下（0.25、2.0和10.0 μg/kg），鸡肉和鸡蛋的平均回收率分别为97.9%～106.0%和97.8%～110.0%，相对标准偏差（RSD）分别为0.9%～6.4%和1.0%～4.7%。结论 该方法简便、灵敏、准确，适用于鸡肉和鸡蛋中5种硝基咪唑残留量的快速检测。
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| 关 键 词： | 硝基咪唑 鸡蛋 鸡肉 超高效液相色谱-串联质谱法 |
Determination of five nitroimidazoles residues in chicken and eggs by ultra performance liquid chromatography-tandem mass spectrometry |
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| LING Li,QU Liang-jiao,LIANG Su-dan,ZHANG Yan.Determination of five nitroimidazoles residues in chicken and eggs by ultra performance liquid chromatography-tandem mass spectrometry[J].Modern Preventive Medicine,2022,0(16):3029-3035. |
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| Authors: | LING Li QU Liang-jiao LIANG Su-dan ZHANG Yan |
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| Affiliation: | Institute of Physical and Chemical Inspection, Zhuhai Center for Disease Control and Prevention, Zhuhai, Guangdong 519060, China |
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| Abstract: | Objective To develop a method of ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the determination of five nitroimidazoles residues in chicken and eggs. Methods The target analytes were extracted with acetonitrile, and then anhydrous Na2SO4 and NaCl were added. After centrifugation, the supernatant was purified using a PRiME HLB SPE cartridge, then the filtrate and acetonitrile eluent were blown to near dryness at 45 ℃ by nitrogen, and finally the residue was redissolved in 10% (v/v) methanol - water. The separation was accomplished on a BEH C18 (2.1 mm × 100 mm, 1.7 μm) column with 0.1% formic acid water and methanol as mobile phase. The analysis was detected in positive electrospray ionization mode under multiple reaction monitoring, and the quantifications were based on the internal standard curves. Results The correlation coefficients of five nitroimidazole were all greater than 0.999 in the range of 0.2 ng/ml to 20.0 ng/ml, with the limits of detection and quantitation of 0.05 μg/kg to 0.1 μg/kg and 0.15 μg/kg to 0.3 μg/kg, respectively. The average recoveries for chicken and eggs were 97.9% to 106.0% and 97.8% to 110.0% for the spiked levels of 0.25 μg/kg, 2.0 μg/kg, and 10.0 μg/kg, respectively, with the relative standard deviations (RSDs) of 0.9% to 6.4% and 1.0 % to 6.7%. Conclusion The proposed method is simple, sensitive, and accurate, and it is suitable for the determination of five nitroimidazoles in chicken and eggs. |
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| Keywords: | Nitroimidazole Egg Chicken Ultra performance liquid chromatography - tandem mass spectrometry (UPLC-MS/MS) |
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