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高效液相色谱-串联质谱法测定动物源性食品中7种苯并咪唑类和2种硝基咪唑类药物残留
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南京海关动植物与食品检测中心

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Determination of residues of seven benzimidazoles and two nitroimidazoles in animal-derived foods by high performance liquid chromatography-tandem mass spectrometry
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Nanjing Customs Animal, Plant and Food Testing Center

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    摘要:

    为同时测定多种基质中7种苯并咪唑类和2种硝基咪唑类药物留量,建立了高效液相色谱-串联质谱法同时检测动物源性食品中三氯苯达唑酮、甲苯咪唑、羟基甲苯咪唑、氨基甲苯咪唑、芬苯达唑、奥芬达唑、奥芬达唑砜、洛硝达唑和替硝唑残留量的方法。样品经盐酸羟胺溶液预处理以保护三氯苯哒唑酮,随后采用酸性乙腈提取,PRiME HLB固相萃取柱净化,采用C18 Core shell色谱柱分离,以甲醇-体积分数0.1%甲酸水溶液为流动相进行梯度洗脱;在电喷雾正离子模式下电离,选择反应监测(Selected Reaction Monitoring,SRM)模式检测,同位素内标法定量。7种苯并咪唑类药物在10-400 ng·mL-1范围内线性关系良好(相关系数R2>0.99),检出限为3 μg·kg-1,定量限为10 μg·kg-1;2种硝基咪唑类药物在1-40 ng·mL-1范围内线性关系良好(相关系数R2>0.99),检出限为0.3 μg·kg-1,定量限为1.0 μg·kg-1。在猪肉、鱼肉、鸡蛋、牛奶和蜂蜜五种基质中进行加标试验,在1、2、10倍定量限添加水平下的平均回收率范围为71.3%~106.4%,相对标准偏差范围为0.6%~9.2%。本方法操作简便、灵敏度高且基质覆盖范围广,可实现动物源性食品中多种苯并咪唑类和硝基咪唑类药物残留量的同步检测,能满足国际上严苛的限量要求,可为进出口食品安全监管工作提供可靠的技术支持。

    Abstract:

    In order to simultaneously detect and quantify the residues of seven benzimidazole and two nitroimidazole drugs in multiple matrices, a method for the simultaneous detection of triclabendazole ketone, mebendazole, hydroxymebendazole, amino mebendazole, fenbendazole, oxfendazole, oxfendazole sulfone, ronidazole and tinidazole residues in animal-derived foods was established by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Samples were pretreated with hydroxylamine hydrochloride solution to protect triclabendazolone, then extracted with acidic acetonitrile, purified on a PRiME HLB solid phase extraction column, separated on a C18 Core shell column with gradient elution using methanol-0.1% formic acid in water as mobile phase. Ionization was performed in electrospray positive ion mode, detection was carried out in selected reaction monitoring mode (Selected Reaction Monitoring, SRM), and quantification was achieved by isotope internal standard method. The seven benzimidazoles showed good linearity in the range of 10–400 ng·mL-1 (correlation coefficients R2 > 0.99) with a limit of quantification (LOQ) of 10 μg·kg-1. The two nitroimidazoles showed good linearity in the range of 1–40 ng·mL-1 (R2 > 0.99) with an LOQ of 1.0 μg·kg-1. Spiked recovery tests were conducted in pork, fish, egg, milk and honey at three levels (1LOQ、2LOQ and 10LOQ). The average recoveries ranged from 71.3% to 106.4%, with relative standard deviations (RSDs) of 0.6%–9.2%. This method features simple operation, high sensitivity and a wide matrix coverage range. It enables the simultaneous detection of residues of multiple benzimidazoles and nitroimidazoles in animal-derived foods, meets the stringent international residue limits, and provides reliable technical support for the food safety supervision of import and export commodities.

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  • 收稿日期:2026-04-23
  • 最后修改日期:2026-07-07
  • 录用日期:2026-07-08
  • 在线发布日期: 2026-11-13
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