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.
作者
张永茂
唐会鑫
李朔
秦江芬
瞿峰
王可
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)
出处
《职业与健康》
CAS
2022年第14期1898-1901,共4页
Occupation and Health
关键词
高效液相色谱串联质谱
酱油
醋
生物胺
High performance liquid chromatography tandem mass spectrometry
Soy sauce
Vinegar
Biogenic amines
