QuEChERS-超高效液相色谱-串联质谱法测定板栗中白僵菌素和恩镰孢菌素
Determination of beauvericin and enniatins in chestnut by QuEChERS-ultra high performance liquid chromatography- tandem mass spectrometry
投稿时间:2025-10-27  修订日期:2025-12-01
DOI:
中文关键词:  白僵菌素  恩镰孢菌素  超高效液相色谱-串联质谱法  板栗
英文关键词:beauvericin  enniatin  ultra high performance liquid chromatography- tandem mass spectrometry  chestnut
基金项目:北京市怀柔区科技计划项目(SHFZ 2020-1)
作者单位
王权帅 北京市怀柔区疾病预防控制中心 
闫乐 北京市怀柔区疾病预防控制中心 
孙卫明 北京市怀柔区疾病预防控制中心 
贾建伟 北京市怀柔区疾病预防控制中心 
刘伟 北京市怀柔区疾病预防控制中心 
袁舜麟 北京市怀柔区疾病预防控制中心 
杜志刚 北京市怀柔区疾病预防控制中心 
陈玲霞 北京市怀柔区疾病预防控制中心 
AuthorInstitution
wang quanshuai Beijing Huairou District Center for Diseases Control and Prevention 
YAN Le Beijing Huairou District Center for Diseases Control and Prevention 
SUN Wei-Ming Beijing Huairou District Center for Diseases Control and Prevention 
JIA Jian-Wei Beijing Huairou District Center for Diseases Control and Prevention 
LIU Wei Beijing Huairou District Center for Diseases Control and Prevention 
YUAN Shun-Lin Beijing Huairou District Center for Diseases Control and Prevention 
DU Zhi-Gang Beijing Huairou District Center for Diseases Control and Prevention 
CHEN Ling-Xia Beijing Huairou District Center for Diseases Control and Prevention 
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中文摘要:
      目的 建立同时测定板栗中白僵菌素( beauvericin,BEA)、恩镰孢菌素A(enniatin A, ENN A)、恩镰孢菌素A1(enniatin A1, ENN A1)、恩镰孢菌素B(enniatin B, ENN B)和恩镰孢菌素B1(enniatin B1, ENN B1)含量的QuEChERS-超高效液相色谱-串联质谱法。 方法 对质谱条件进行优化,通过比较选择最佳的色谱柱和流动相条件,通过回收率指标确定最优的提取试剂和QuEChERS净化柱,分析板栗样本对5种新兴真菌毒素的基质效应。最后对建立的方法进行方法学实验。结果 该方法最终使用乙腈-水(80+20)对试样进行提取,使用QuEChERS净化柱(PSA 50mg,MgSO4 150 mg)进行净化处理。采用BEH C18为分析色谱柱,流动相为乙腈- 2 mmoL/L乙酸铵溶液。方法的基质效应不能忽略,应采用内标法进行定量分析,BEA、ENN A、ENN A1、ENN B和ENN B1的检出限为0.03 μg/kg,定量限为0.1 μg/kg,回收率为97.7%~117.7%之间,相对标准偏差为1.6%~8.4%,相关系数均≥0.9990。结论 本方法操作简便快捷,准确度和灵敏度高,适用于板栗中BEA、ENN A、ENN A1、ENN B和ENN B1的同时测定。
英文摘要:
      Objective Establish an QuEChERS ultra high performance liquid chromatography tandem mass spectrometry method for simultaneous determination of the content of beauvericin (BEA), enniatin A (ENN A), enniatin A1 (ENN A1), enniatin B (ENN B) and enniatin B1 (ENN B1) in chestnuts. Methods Determine the optimal mass spectrometry conditions for 5 target mycotoxins through parameter optimization, select the best liquid chromatographic column and mobile phase through comparative experiments, confirm the optimal extraction reagent and QuEChERS purification column through recovery rate, analyze matrix effect of chestnut on these 5 emerging mycotoxins. Finally, conduct methodological experiments on the established method. Results The method ultimately used acetonitrile- water (80+20) as the extraction reagent for sample pretreatment, selected QuEChERS column (PSA 50mg, MgSO4 150 mg) for cleaning Treatment. The BEH C18 column was used as the chromatographic column and acetonitrile- 2 mmoL/L ammonium acetate was used as the mobile phase. The matrix effect of the method cannot be ignored, the internal standard method should be used for quantitative analysis. The detection limits of BEA、ENN A、ENN A1、ENN B and ENN B1 were 0.03 μg/kg and the quantification limits were 0.1 μg/kg. The recovery rate was between 97.7% and 117.7%, the relative standard deviation was 1.6% to 8.4%, the correlation coefficients were all ≥ 0.9990. Conclusion This method is simple, rapid, with the high accurates and ensitivity, which could be used for simultaneous determination of the content of BEA、ENN A、ENN A1、ENN B and ENN B1 .
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