固相萃取-超高效液相色谱串联质谱法同时测定豆芽中6-苄基腺嘌呤、赤霉素和4-氯苯氧乙酸的残留量
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(河北出入境检验检疫局,河北 石家庄 050051)

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张婧雯 女 工程师 研究方向为食品安全分析检测 E-mail:jingwen0415@163.com通讯作者:┣┣(中)通信作者┫┫艾连峰 男 高级工程师 研究方向为食品安全分析检测E-mail:ai_lianfeng@126.com

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国家质检总局科技计划项目(2013IK154);河北检验检验局科研项目(HE2011K005)


Simultaneous determination of 6-benzylaminopurine, gibberellin and 4-chlorophenoxyacetic acid in bean sprouts by solid phase extractionultra high performance liquid chromatography tandem mass spectrometry
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(Hebei Entry-Exit Inspection and Quarantine Bureau,Shijiazhuang 050051,China)

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    摘要:

    建立固相萃取-超高效液相色谱串联质谱同时测定豆芽中6-苄基腺嘌呤、赤霉素和4-氯苯氧乙酸残留的分析方法。方法 以乙腈提取目标物,HLB固相萃取柱(3 ml/600 mg)净化提取液,以0.1%甲酸水和乙腈为流动相,采用ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7 μm)分离,液相色谱串联质谱采用正负离子同时扫描、多反应监测模式测定。结果 3种分析物在0.1~20 μg/L浓度范围内呈线性,线性相关系数(r)>0.99。方法定量限(LOQ)为0.5 μg/kg。方法在3个水平的添加回收率在70.1%~93.5%之间,RSD在5.01%~9.34%之间。结论 本方法具有快速、灵敏、简便、准确等优点,能满足实际工作需要。

    Abstract:

    To establish an ultra high performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) method for the simultaneous determination of 6-benzylaminopurine, gibberellins and 4-chlorophenoxyacetic acid residues in bean sprouts. MethodsThe samples were extracted with acetonitrile. The extract was cleaned up by a HLB solid phase column. The target compounds were separated by ACQUITY UPLC BEH C18Column (100 mm×2.1 mm, 1.7 μm) with 0.1% formic acid and acetonitrile as the mobile phase, and then analyzed by ultra high performance liquid chromatography using positive and negative simultaneous scan mode and multiple reactions monitoring mode. ResultsThe linearity was satisfactory at concentrations ranging from 0.1 to 20 μg/L with linear correlation coefficient(r2)above 0.99.The limit of quantification (LOQ) was 0.5 μg/kg.The recoveries of the 3 analytes were in the range of 70.1% to 93.5%, and the relative standard deviations were in the range of 5.01% to 9.34%.ConclusionThis method was sensitive, fast and accurate. Therefore, it couldbe successfully used for the determination of 6-benzylaminopurine, gibberellins and 4-chlorophenoxyacetic acid residues in bean sprouts.

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张婧雯,郭春海,葛世辉,张海超,王敬,窦彩云,艾连峰.固相萃取-超高效液相色谱串联质谱法同时测定豆芽中6-苄基腺嘌呤、赤霉素和4-氯苯氧乙酸的残留量[J].中国食品卫生杂志,2014,26(5):441-445.

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  • 收稿日期:2013-11-13
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  • 在线发布日期: 2014-10-16
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