酱油和醋中8种生物胺的高效液相色谱串联质谱测定法  

Determination of eight kinds of biogenic amines in soy sauce and vinegar by high performance liquid chromatography tandem mass spectrometry

作　　者：张永茂[1] 唐会鑫 李朔 秦江芬 瞿峰 王可[2] ZHANG Yong-mao;TANG Hui-xin;LI Shuo;QIN Jiang-fen;QU Feng;WANG Ke(Research and Training Department,Hebei Provincial Center for Disease Control and Prevention,Shijiazhuang Hebei,050021,China;Shijiazhuang Technology Innovation Center for Chemical Poison Detection and Risk Early Warning,Shijiazhuang Center for Disease Control and Prevention,Shijiazhuang Hebei,050011,China;Cancer Institute,Fourth Hospital of Hebei Medical University,Shijiazhuang Hebei,050011,China)

机构地区：[1]河北省疾病预防控制中心科研培训处,河北石家庄050021 [2]石家庄市疾病预防控制中心,石家庄市化学毒物检测及风险预警技术创新中心,河北石家庄050011 [3]河北医科大学第四医院肿瘤研究所,河北石家庄050011

出　　处：《职业与健康》2022年第14期1898-1901,共4页Occupation and Health

摘　　要：目的 改进前处理过程,建立可用于开展酱油、醋中8种生物胺检测的高效液相色谱串联质谱(high performance liquid chromatography tandem mass spectrometry,HPLS-MS/MS)法。方法 采用1.0 mol/L盐酸酸化样品,经正丁醇-三氯甲烷(4∶6,v/v)的混合液超声提取后,氮吹近干。用0.02 mol/L盐酸复溶,经0.22μm滤膜过滤后,用HC-C18(4.6×250 mm,5μm)色谱柱分离,HPLC-MS/MS检测。结果 在比较宽的浓度范围(0.5~5 000 ng/mL)内,线性良好(r≥0.999),定量限各有不同,范围在0.04~1.78 mg/kg之间,不同加标浓度下的回收率为64.4%~111.1%,相对标准偏差(relative stardard deviation,RSD)为0.5%~5.2%。结论 所建立的方法具有快速、灵敏、精准等优点,适合于酱油和醋中生物胺的风险监测工作。Objective Based on pretreatment improvement,to establish a new high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS) method for detecting eight biogenic amines in soy sauce and vinegar. Methods After acidified by 1.0 mol/L hydrochloric acid,the biogenic amines were extracted from the samples with the mixed solution of n-butanol and chloroform(4∶6,v/v) under ultrasonic oscillation. The supernatant were dried by nitrogen,then the extract was dissolved in0.02 mol/L hydrochloric acid,filtered with 0.22 μm filter membrane,analyzed on HC-C18 column(4.6×250 mm,5 μm),and tested by HPLC-MS/MS. Results In a wide range of concentrations(0.5-5 000 ng/mL),the good linearity was achieved with significant correlations(r≥0.999). The limits of quantitation were in the range of 0.04-1.78 mg/kg. For different spiked concentration,the recoveries were from 64.4% to 111.1%,and the relative standard deviation(RSD) was 0.5%-5.2%. Conclusion This method has the advantages including rapid,sensitive and accurate,which is proper to promote the risk surveillance of biogenic amines in soy sauce and vinegar.

关 键 词：高效液相色谱串联质谱 酱油 醋 生物胺 

分 类 号：R115[医药卫生—公共卫生与预防医学]