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作 者:缪琼惠 张志清 闵向东[3] 段志敏[3] 李承蹊 林佶[3] MIAO Qiong-Hui;ZHAN Zhi-Qing;MIN Xiang-Dong;DUAN Zhi-Min;LI CHENG-Xi;LIN Ji(School of Public Health,Dali University,Dali 671000,China;School of Public Health,Kunming Medical University,Kunming 650500,China;Yunnan Center for Disease Control and Prevention,Kunming 650032,China)
机构地区:[1]大理大学公共卫生学院,大理671000 [2]昆明医科大学公共卫生学院,昆明650500 [3]云南省疾病预防控制中心,昆明650032
出 处:《食品安全质量检测学报》2021年第13期5299-5305,共7页Journal of Food Safety and Quality
摘 要:目的建立高效液相色谱-三重四极杆质谱法快速检测鱼腥草中9种马兜铃酸类物质的分析方法。方法采用A CQUITY UPLC®HSS T3色谱柱(100 mm×2.1 mm,1.8μm),0.1%甲酸-5 mmol/L-水溶液(A)及甲醇(B)为流动相,梯度洗脱,流速为0.35 mL/min,柱温为40℃,采用正离子多反应监测模式进行检测。结果9种马兜铃酸类物质在线限范围内线性关系良好(r>0.9990),平均加样回收率(n=6)为89.62%~107.61%,相对标准差≤5.18%。此批鱼腥草样品中马兜铃酸(A、B、C、D)、7-羟基马兜铃酸A、马兜铃内酰胺、马兜铃酮均未检出,马兜铃内酰胺F1含量最低值为0.376 mg/kg,含量最高值为7.034 mg/kg;马兜铃内酰胺BII含量最低值为0.984 mg/kg,含量最高值为11.931 mg/kg。结论此方法灵敏度高、可重复性好、回收率较高、操作简便、效率高,适用于鱼腥草中多种马兜铃酸类化合物的检测。Objective To establish a method for the determination of 9 kinds of ristolochic acids in Houttuynia cordata by high performance liquid chromatography-triple quadrupole mass spectrometry.Methods A CQUITY UPLC®HSS T3 column(100 mm×2.1 mm,1.8μm)was used,0.1%formic acid-5 mmol/L-aqueous solution(A)and methanol(B)were used as mobile phases,gradient elution was carried out,the flow rate was 0.35 mL/min,the column temperature was 40℃,and the positive ion multi-reaction monitoring mode was used for detection.Results The linear range of 9 aristolochic acids was good(r>0.9990),and the average recoveries(n=6)were 89.61%-107.61%,relative standard deviation≤5.18%.Aristolochic acid(A,B,C,D),7-hydroxyaristolochic acid A,aristolochic lactam and aristolochic ketone in this batch of Houttuynia cordata samples were not detected.The lowest content of aristolochic lactam F1 was 0.376 mg/kg,and the highest content was 7.034 mg/kg.The lowest content of aristolochia lactam BII was 0.984 mg/kg,and the highest content was 11.931 mg/kg.Conclusion This method has high sensitivity,good repeatability,high recovery rate,simple operation and high efficiency,which is suitable for the detection of various aristolochic acids in Houttuynia cordata samples.
关 键 词:高效液相色谱-串联质谱法 马兜铃酸类物质 鱼腥草
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