超高效液相色谱-串联质谱法检测水产品中的丁香酚  

Determination of eugenol in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：胡潇潇 杨妍 董宁宁 刘静 程名玉 HU Xiaoxiao;YANG Yan;DONG Ningning;LIU Jing;CHENG Mingyu(Institute of Physical and Chemical Laboratory,Zhengzhou Center for Disease Control and Prevention,Zhengzhou,Henan 450000,China)

机构地区：[1]郑州市疾病预防控制中心理化检验所,河南郑州450000

出　　处：《职业与健康》2025年第4期453-457,共5页Occupation and Health

摘　　要：目的 建立超高效液相色谱-四极杆质谱法检测水产品中丁香酚残留量的方法。方法 鱼肉和虾肉样品经乙腈超声提取,HLB固相萃取柱净化,氮吹富集浓缩后用25%甲醇水溶液定容,离心过膜。以甲醇-0.01%氨水为流动相进行梯度洗脱,经Kromasil EternityXT-2.5-PhenylHexy(2.1 mm×100 mm,1.7μm)色谱柱分离,在多反应监测模式(multiple reaction monitoring,MRM)负离子状态下检测,内标法定量。结果 丁香酚在2.0~200μg/L范围内线性关系良好(r≥0.999),方法检出限在1.0μg/kg,定量限为2.5μg/kg,低、中、高3个加标水平(2.5、7.5、100μg/kg)下的平均回收率(n=6)在98.0%~107.0%之间,精密度(n=6)在1.70%~7.07%之间。利用此方法对30份鱼虾样品进行检测,检出率为40%,鱼产品中检出率为75%,虾产品中检出率为0。结论 所建立的方法操作简单、快速,且定量结果准确可靠,可以实现在短时间内对水产品中丁香酚的检测。Objective To establish a method for detecting residual eugenolin aquatic products using ultra high performance liquid chromatography quadrupole mass spectrometry. Methods Fish and shrimp meat samples were ultrasonically extracted with acetonitrile at room temperature,purified by HLB solid-phase extraction column,enriched concentrated by nitrogen flushing,and then diluted with 25% methanol aqueous solution and centrifuged through a membrane. Gradient elution was performed using methanol-0.01% ammonia solution as the mobile phase,and separated by Kromasil Eternity XT-2.5-PhenylHexy(2.1 mm×100 mm,1. 7 μm) chromatographic column. The detection was performed in multiple reaction monitoring(MRM) mode with negative electrospray ionization and quantified by internal standard method. Results The linear relationship of eugenol was good within the range of 2.0-200 μg/L(r≥0.999). The detection limit of the method was 1.0 μg/kg,and the quantification limit was 2.5 μg/kg.The average recoveries(n=6) at low,medium,and high spiked levels(2.5,7.5,and 100 μg/kg) was between 98.0% and 107.0%,and the precision(n=6) was between 1.70% and 7.07%. Using this method,30 fish and shrimp samples were tested with a detection rate of 40%. The detection rate in fish products was 75%,and the detection rate in shrimp products was 0. Conclusion The established method is simple and fast to operate,and the quantitative results are accurate and reliable,which can achieve the detection of eugenol in aquatic products in a short period of time.

关 键 词：超高效液相色谱-四级杆-质谱 丁香酚 水产品 

分 类 号：R115[医药卫生—公共卫生与预防医学]