高效液相色谱—串联质谱法测定猪可食性组织中烯丙孕素残留
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(1. 北京市农产品质量安全中心,北京 102629;2. 安徽中医药大学,安徽 合肥 230012)

作者简介:

倪香艳,女,北京市农产品质量安全中心兽医师,硕士。

通讯作者:

孙志文(1976—),男,北京市农产品质量安全中心高级兽医师,硕士。E-mai: Sunzw673@163.com

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安徽省高等学校科学研究项目(编号:KJ2021A0593)


Determination of altrenogest residue in pig edible tissue by a high performance liquid chromatography-tandem mass spectrometry method
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(1. Beijing Agricultural Product Quality and Safety Center, Beijing 102629, China;2. Anhui University of Chinese Medicine, Hefei, Anhui 230012, China)

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    摘要:

    目的:测定猪可食性组织(肌肉、肝脏、脂肪)中烯丙孕素残留。方法:试样经β-葡萄糖醛酸酶/芳基硫酸酯酶酶解,乙腈提取,PRiME HLB固相萃取柱净化。以乙腈—0.1%甲酸水溶液作为流动相,经Waters UPLC BEH C18反相色谱柱分离后于电喷雾正离子模式下检测,基质匹配外标法定量。结果:烯丙孕素在1~50 μg/L的质量浓度范围内线性良好,线性相关系数R2 >0.99;该方法在猪肌肉、肝脏、脂肪组织中检测限为0.5 μg/kg,定量限为1.0 μg/kg。在3个添加水平下(1.0,2.0,10.0 μg/kg),平均回收率为60.9%~89.8%,日内变异系数为0.8%~7.1%,日间变异系数为2.5%~11.6%。结论:该方法操作简便,适用于猪可食性组织中烯丙孕素残留的定性与定量分析。

    Abstract:

    Objective: To determinate the residues of altrenogest in porcine edible tissues (muscle, liver, fat), a high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was established. Methods: The samples were hydrolyzed with β-glucuronidase/arylsulfase, extracted by acetonitrile (ACN), purified by PRiME HLB solid phase extraction column. LC separation was performed with Waters UPLC BEH C18 reversed-phase chromatography with a linear gradient elution of acetonitrile (ACN)-0.1% formic acid (FA) as the mobile phase. The samples were detected by electrospray in positive ion mode. Results: The pregnancin in tissues were quantified in the range of 1~50 μg/L with good linearity and high linear correlation coefficient (R2>0.99). The limit of detection (LOD, S/N=3) and the limit of quantification (LOQ, S/N=10) were as low as 0.5 μg/kg and 1.0 μg/kg separately. Under three different concentrations (1.0, 2.0, 10.0 μg/kg), the average recoveries were 60.9%~89.8%, the intra-day coefficient of variation was 0.8%~7.1%, and the inter-day coefficient of variation was 2.5%~11.6%. Conclusion: The method is simple and suitable for the qualitative and quantitative analysis of altrenogest residue in porcine edible tissues.

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倪香艳,孙念霞,于寒冰,等.高效液相色谱—串联质谱法测定猪可食性组织中烯丙孕素残留[J].食品与机械,2023,39(2):45-49.
NI Xiang-yan, SUN Nian-xia, YU Han-bing, et al. Determination of altrenogest residue in pig edible tissue by a high performance liquid chromatography-tandem mass spectrometry method[J]. Food & Machinery,2023,39(2):45-49.

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  • 收稿日期:2022-06-21
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  • 在线发布日期: 2023-04-25
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