摘要
建立了一种氟虫腈及其代谢物氟虫腈砜标准物质候选物中的主要有机杂质定性、定量分析方法。采用高效液相色谱-三重四极杆串联质谱法(HPLC-MS/MS)成功鉴别出氟虫腈中杂质分别为氟虫腈砜和氟虫腈硫化物,而氟虫腈砜中杂质为氟虫腈硫化物,推导出氟虫腈砜的结构式。HPLC-MS/MS外标法测定氟虫腈中杂质氟虫腈砜和氟虫腈硫化物的含量分别为0. 18%、0. 47%,相对标准偏差分别为0. 73%、0. 87%;氟虫腈砜中杂质氟虫腈硫化物的含量为0. 25%,相对标准偏差为8. 05%。该方法的研究对食品安全检验中氟虫腈及氟虫腈砜的准确测定具有重要意义。
Qualitative and quantitative analysis of the major organic impurities in pure fipronil and its metabolite fipronil sulfone was performed.The organic impurities were qualitatively determined by high performance liquid chromatography-triple quarupole tandem mass spectrometry( HPLC-MS/MS).Full scan of LC/MS in positive ion mode was firstly executed to obtain the m/z values of the molecules.Then LC-MS/MS was carried out on target compounds to obtain structural information.Impurities in fipronil were successfully identified as fipronil sulfone and fipronil sulphide,respectively. The molecular structure of fipronil sulfone was derived and impurity in fipronil sulfone was successfully identified as fipronil sulphide. HPLC-MS/MS external standard method was used to determine the content of the organic impurities.There are 0. 18% fipronil sulfone with the RSD of 0. 73% and 0. 47%fipronil sulphide with the RSD of 0. 87% in pure fipronil material.The content of impurity in fipronil sulfone material was 0. 25%with the RSD of 8. 05%. Moreover,this method has instructive significance to the qualitative and quantitative analysis of pure fipronil and fipronil sulfone and other pure organic substances.
引文
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