| 双氯芬酸钠残留检测的质谱条件选择 |
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| 引用本文： | 杨亚军,刘希望,秦 哲,李世宏,焦增华,李剑勇.双氯芬酸钠残留检测的质谱条件选择[J].西北农业学报,2019,28(9):1403-1410. |
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| 作者姓名： | 杨亚军 刘希望 秦 哲 李世宏 焦增华 李剑勇 |
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| 作者单位： | （中国农业科学院 兰州畜牧与兽药研究所，农业部兽用药物创制重点实验室，甘肃省新兽药工程重点实验室，兰州 730050） |
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| 基金项目： | 中国农业科学院农业科技创新工程（CAAS-ASTIP-2014-LIHPS-2）。 |
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| 摘 要： | 为优化双氯芬酸(DCF)残留检测过程中的质谱参数,提高其检测灵敏度。在电喷雾离子源负离子(ESI~-)和正离子(ESI~+)模式下,分别对DCF标准溶液进行母离子和子离子扫描,以优化定量检测的参数;比较ESI~-和ESI~+条件下,标准溶液和空白肝脏加标样品定量离子的响应。结果显示,在ESI~-模式下,DCF存在明显的源内裂解现象,而ESI~+模式下则未出现类似现象;因此导致质量浓度为2 ng/mL的DCF标准溶液在ESI~-条件下定量离子的峰面积远低于ESI~+;ESI~-条件下,空白肝脏加标样品(0.5 ng/g,LOQ)中几乎检测不到定量离子,而ESI~+条件下定量离子的响应则可满足检测要求。鉴于DCF在ESI~-条件下可发生源内裂解,建议在DCF的残留检测中采用ESI~+模式。
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| 关 键 词： | 双氯芬酸钠 残留检测 LC-MS/MC 源内裂解 |
Mass Spectrometry Condition Selection in Residue Determination of Diclofenac Sodium |
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| YANG Yajun,LIU Xiwang,QIN Zhe,LI Shihong,JIAO Zenghua and LI Jianyong.Mass Spectrometry Condition Selection in Residue Determination of Diclofenac Sodium[J].Acta Agriculturae Boreali-occidentalis Sinica,2019,28(9):1403-1410. |
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| Authors: | YANG Yajun LIU Xiwang QIN Zhe LI Shihong JIAO Zenghua and LI Jianyong |
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| Abstract: | To increase liquid chromatography tandem mass spectrometry (LC-MS/MS) determination sensitivity,MS condition of diclofenac acid (DCF) was optimized in the present paper. Standard solutions of DCF and internal standard (IS,13C-DCF) were scanned with precursor ion and product ion modes by electrospray ionization (ESI) source interface operated in the negative and positive-ion scan modes,respectively. Then,the parameters for multiple-reaction monitoring (MRM) were optimized,and the characteristical ions of DCF and IS were selected. The peak areas of quantifier ion were compared when the standard solution and the blank liver samples spiked with DCF and IS were determined through MRM with ESI- and ESI+,respectively. Conversion in-source of DCF was observed in ESI- mode,but not in ESI+ mode. As the conversion in-source,the peak area of quantifier ion of 2 ng/mL standard solution with ESI- was much lower than ESI+. The peak of quantifier ion in blank liver samples spiked with DCF(0.5 ng/g,LOQ) was almost not found under ESI- mode. However,the results of the samples were accordance to the determination requirements under ESI+ mode. The results suggested that ESI+ mode should be used in DCF residue determination,because there was conversion in-source of DCF in ESI- mode. |
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| Keywords: | Diclofenac sodium Residue determination LC-MS/MS Conversion in-source |
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