食品科学 ›› 2023, Vol. 44 ›› Issue (14): 360-367.doi: 10.7506/spkx1002-6630-20220715-177

• 安全检测 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定动物源性食品中的13 种利尿剂

任晓伟,范力欣,何亮娜,孙磊,马俊美   

  1. (河北省食品安全重点实验室,国家市场监管重点实验室(特殊食品监管技术),特殊食品安全与健康河北省工程研究中心,河北省食品检验研究院,河北?石家庄 050000)
  • 出版日期:2023-07-25 发布日期:2023-08-11
  • 基金资助:
    河北省技术创新引导计划项目(21475501D)

Determination of 13 Diuretics in Animal-Derived Foods by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

REN Xiaowei, FAN Lixin, HE Liangna, SUN Lei, MA Junmei   

  1. (Hebei Food Safety Key Laboratory, Key Laboratory of Special Food Supervision Technology for State Market Regulation, Hebei Engineering Research Center for Special Food Safety and Health, Hebei Food Inspection and Research Institute, Shijiazhuang 050000, China)
  • Online:2023-07-25 Published:2023-08-11

摘要: 使用超高效液相色谱-串联质谱建立测定动物源性食品中13 种利尿剂的方法。样品经乙腈或90%乙腈溶液提取和PRiME HLB通过式固相萃取柱净化后使用ACQUITY HSS T3色谱柱(100 mm×2.1 mm,1.8 μm)分离,流动相分别为乙腈和5 mmol/L乙酸铵溶液,梯度洗脱。在电喷雾正/负离子同时扫描的模式下进行定性和定量的检测。结果表明:13 种利尿剂线性关系良好,相关系数均达0.997 0以上。定量限范围为2.0~5.0 μg/kg。方法回收率范围为68.3%~118.0%,相对标准偏差为0.47%~9.5%(n=6)。本方法简便准确,实用性强,可用于对利尿剂的快捷、精准检测。

关键词: 超高效液相色谱-串联质谱;利尿剂;固相萃取柱;动物源性食品

Abstract: A novel efficient and accurate ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the detection of 13 diuretics in animal-derived foods was developed. The samples were extracted with acetonitrile or 90% acetonitrile solution and cleaned up on a PRiME HLB pass-through solid phase extraction (SPE) column. Then, an ACQUITY HSS T3 column (100 mm × 2.1 mm, 1.8 μm) was used for chromatographic separation by gradient elution using a mobile phase consisting of 5 mmol/L aqueous ammonium acetate and acetonitrile, and an electrospray ionization source (ESI) operated in both positive and negative ion scanning modes with multiple reaction monitoring (MRM) was used to detect the diuretics qualitatively and quantitatively. The results showed that the calibration curves for all the analytes exhibited good linearity with correlation coefficients above 0.997 0. The limits of quantification ranged from 2.0 to 5.0 μg/kg. The recoveries of the proposed method ranged between 68.3% and 118.0%, with relative standard deviations (RSDs) between 0.47% and 9.5% (n = 6). This method is a fast, simple, accurate, and practical one for the detection of diuretics.

Key words: ultra-high performance liquid chromatography-tandem mass spectrometry; diuretics; solid phase extraction cartridge; animal-derived foods

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