高效液相色谱-串联质谱法测定玉米中虫酰肼残留量
目的建立高效液相色谱-串联质谱法检测玉米中虫酰肼的残留量。方法样品经含1%乙酸的乙腈溶液提取,再经N-丙基乙二胺（PSA）、石墨化炭黑和十八烷基硅烷（octadecylsilane,ODS）净化,用ACQUITY UPLC BEH C18（100 mm×2.1 mm,1.7μm）柱分离,以0.1%乙酸水溶液和乙腈作为流动相进行梯度洗脱,然后经质谱法检测,以外标法定量。结果虫酰肼在4100 ng/m L浓度范围内时,线性关系良好,相关系数为0.9933。在0.001、0.05和25.0 mg/kg 3个水平加标的平均加标回收率为85.5%105.0%之间,相对标准偏差均小于10.1%,检出限为0...
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| Published in | 食品安全质量检测学报 Vol. 8; no. 2; pp. 416 - 420 |
|---|---|
| Main Author | |
| Format | Journal Article |
| Language | Chinese |
| Published |
黑河出入境检验检疫局,黑河,164300%黑龙江出入境检验检疫局,哈尔滨,150001%同江出入境检验检疫局,佳木斯,156499
2017
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| Subjects | |
| Online Access | Get full text |
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| Abstract | 目的建立高效液相色谱-串联质谱法检测玉米中虫酰肼的残留量。方法样品经含1%乙酸的乙腈溶液提取,再经N-丙基乙二胺（PSA）、石墨化炭黑和十八烷基硅烷（octadecylsilane,ODS）净化,用ACQUITY UPLC BEH C18（100 mm×2.1 mm,1.7μm）柱分离,以0.1%乙酸水溶液和乙腈作为流动相进行梯度洗脱,然后经质谱法检测,以外标法定量。结果虫酰肼在4100 ng/m L浓度范围内时,线性关系良好,相关系数为0.9933。在0.001、0.05和25.0 mg/kg 3个水平加标的平均加标回收率为85.5%105.0%之间,相对标准偏差均小于10.1%,检出限为0.001 mg/kg。结论本方法灵敏准确、操作简便,可适用于玉米中虫酰肼残留量的测定。 |
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| AbstractList | 目的 建立高效液相色谱-串联质谱法检测玉米中虫酰肼的残留量.方法 样品经含1%乙酸的乙腈溶液提取,再经N-丙基乙二胺(PSA)、石墨化炭黑和十八烷基硅烷(octadecylsilane,ODS)净化,用ACQUITY UPLC BEH C18(100 mm×2.1 mm,1.7μm)柱分离,以0.1%乙酸水溶液和乙腈作为流动相进行梯度洗脱,然后经质谱法检测,以外标法定量.结果 虫酰肼在4~100 ng/mL浓度范围内时,线性关系良好,相关系数为0.9933.在0.001、0.05和25.0 mg/kg 3个水平加标的平均加标回收率为85.5%~105.0%之间,相对标准偏差均小于10.1%,检出限为0.001 mg/kg.结论 本方法灵敏准确、操作简便,可适用于玉米中虫酰肼残留量的测定. 目的建立高效液相色谱-串联质谱法检测玉米中虫酰肼的残留量。方法样品经含1%乙酸的乙腈溶液提取,再经N-丙基乙二胺（PSA）、石墨化炭黑和十八烷基硅烷（octadecylsilane,ODS）净化,用ACQUITY UPLC BEH C18（100 mm×2.1 mm,1.7μm）柱分离,以0.1%乙酸水溶液和乙腈作为流动相进行梯度洗脱,然后经质谱法检测,以外标法定量。结果虫酰肼在4100 ng/m L浓度范围内时,线性关系良好,相关系数为0.9933。在0.001、0.05和25.0 mg/kg 3个水平加标的平均加标回收率为85.5%105.0%之间,相对标准偏差均小于10.1%,检出限为0.001 mg/kg。结论本方法灵敏准确、操作简便,可适用于玉米中虫酰肼残留量的测定。 |
| Abstract_FL | Objective To establish a method for detection of worm tebufenozide residue in corn by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).Methods Tebufenozide residue in the sample was extracted with acetonitrile containing 1% acetic acid, cleaned up with N-propyl ethylenediamine (PSA), graphitized carbon black and octadecylsilane (ODS), separated by an ACQUITY UPLC BEH C18 column (100 mm×2.1 mm, 1.7μm) using 0.1% acetic acid water solution-acetonitrile as mobile phase for gradient elution, and then detected by tandem mass spectrometry with external standard method for quantification.Results Tebufenozide had a good linearity in the range of 4~100 ng/mL, with a correlation coefficient of 0.9933. The average recoveries of tebufenozide spiked in 3 levels of 0.001, 0.05 and 25.0 mg/kg were ranged from 85.5% to105.0%, with the relative standard deviations below 10.1%. The limit of detection was 0.001 mg/kg.Conclusion This method is sensitive, accurate and simple, which is suitable for the detection of tebufenozide residue in corn. |
| Author | 吕鹏 田丰 宋文成 杨长志 刘巍 |
| AuthorAffiliation | 黑河出入境检验检疫局,黑河164300 黑龙江出入境检验检疫局,哈尔滨150001 同江出入境检验检疫局,佳木斯156499 |
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| Author_FL | LIU Wei TIAN Feng SONG Wen-Cheng YANG Chang-Zhi LV Peng |
| Author_FL_xml | – sequence: 1 fullname: LV Peng – sequence: 2 fullname: TIAN Feng – sequence: 3 fullname: SONG Wen-Cheng – sequence: 4 fullname: YANG Chang-Zhi – sequence: 5 fullname: LIU Wei |
| Author_xml | – sequence: 1 fullname: 吕鹏 田丰 宋文成 杨长志 刘巍 |
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| DocumentTitleAlternate | Determination of tebufenozide residue in corn by high performance liquid chromatography-tandem mass spectrometry |
| DocumentTitle_FL | Determination of tebufenozide residue in corn by high performance liquid chromatography-tandem mass spectrometry |
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| Keywords | tebufenozide 玉米 虫酰肼 corn high performance liquid chromatography-tandem mass spectrometry 高效液相色谱-串联质谱法 |
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| Notes | LV Peng1, TIAN Feng1, SONG Wen-Cheng1, YANG Chang-Zhi2, LIU Wei3 （1. Heihe Entry-Exit Inspection and Quarantine Bureau, Heihe 164300, China;2. Heilongjiang Entry-Exit Inspection and Quarantine Bureau, Harbin 150001, China; 3. Tongjiang Entry-Exit Inspection and Quarantine Bureau, Jiamusi 156499, China） Objective To establish a method for detection of worm tebufenozide residue in corn by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）. Methods Tebufenozide residue in the sample was extracted with acetonitrile containing 1% acetic acid, cleaned up with N-propyl ethylenediamine（PSA）, graphitized carbon black and octadecylsilane（ODS）, separated by an ACQUITY UPLC BEH C18 column（100 mm×2.1 mm, 1.7 μm） using 0.1% acetic acid water solution-acetonitrile as mobile phase for gradient elution, and then detected by tandem mass spectrometry with external standard method for quantification. Results Tebufenozide had a good linearity in the range of 4100 ng/m L, with a correlation coefficient of 0 |
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| PublicationTitle | 食品安全质量检测学报 |
| PublicationTitleAlternate | Journal of Food Safety and Quality |
| PublicationTitle_FL | Journal of Food Safety & Quality |
| PublicationYear | 2017 |
| Publisher | 黑河出入境检验检疫局,黑河,164300%黑龙江出入境检验检疫局,哈尔滨,150001%同江出入境检验检疫局,佳木斯,156499 |
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| Snippet | 目的建立高效液相色谱-串联质谱法检测玉米中虫酰肼的残留量。方法样品经含1%乙酸的乙腈溶液提取,再经N-丙基乙二胺（PSA）、石墨化炭黑和十八烷基硅烷（octadecylsilane,ODS）净化,用ACQUITY UPLC BEH C18（100 mm×2.1... 目的 建立高效液相色谱-串联质谱法检测玉米中虫酰肼的残留量.方法 样品经含1%乙酸的乙腈溶液提取,再经N-丙基乙二胺(PSA)、石墨化炭黑和十八烷基硅烷(octadecylsilane,ODS)净化,用ACQUITY UPLC BEH C18(100 mm×2.1... |
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| SubjectTerms | 玉米 虫酰肼 高效液相色谱-串联质谱法 |
| Title | 高效液相色谱-串联质谱法测定玉米中虫酰肼残留量 |
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