Analytical and Bioanalytical Chemistry ( IF 3.8 ) Pub Date : 2018-03-20 , DOI: 10.1007/s00216-018-1002-1 Kazuhiko Akutsu , Yoko Kitagawa , Masato Yoshimitsu , Satoshi Takatori , Naoki Fukui , Masakazu Osakada , Kotaro Uchida , Emiko Azuma , Keiji Kajimura
Polyethylene glycol 300 is commonly used as a base material for “analyte protection” in multiresidue pesticide analysis via gas chromatography-mass spectrometry. However, the disadvantage of the co-injection method using polyethylene glycol 300 is that it causes peak instability in α-cyano pyrethroids (type II pyrethroids) such as fluvalinate. In this study, we confirmed the instability phenomenon in type II pyrethroids and developed novel analyte protectants for acetone/n-hexane mixture solution to suppress the phenomenon. Our findings revealed that among the examined additive compounds, three lipophilic ascorbic acid derivatives, 3-O-ethyl-L-ascorbic acid, 6-O-palmitoyl-L-ascorbic acid, and 6-O-stearoyl-L-ascorbic acid, could effectively stabilize the type II pyrethroids in the presence of polyethylene glycol 300. A mixture of the three ascorbic acid derivatives and polyethylene glycol 300 proved to be an effective analyte protectant for multiresidue pesticide analysis. Further, we designed and evaluated a new combination of analyte protectant compounds without using polyethylene glycol or the troublesome hydrophilic compounds. Consequently, we obtained a set of 10 medium- and long-chain saturated fatty acids as an effective analyte protectant suitable for acetone/n-hexane solution that did not cause peak instability in type II pyrethroids. These analyte protectants will be useful in multiresidue pesticide analysis by gas chromatography-mass spectrometry in terms of ruggedness and reliable quantitativeness.
中文翻译:
气相色谱-质谱法在多残留农药分析中聚乙二醇共注入方法的问题和解决方案:评估II型拟除虫菊酯的不稳定性现象及其新型分析物保护剂的抑制作用
聚乙二醇300通常用作通过气相色谱-质谱法在多残留农药分析中进行“分析物保护”的基础材料。然而,使用聚乙二醇300的共注射方法的缺点在于,它引起α-氰基拟除虫菊酯(II型拟除虫菊酯)例如氟维林酸酯的峰不稳定性。在这项研究中,我们证实了不稳定的现象在II型拟除虫菊酯和开发新颖分析保护为丙酮/ Ñ己烷混合物溶液以抑制的现象。我们的发现表明,在所研究的添加剂化合物中,三种亲脂性抗坏血酸衍生物,3 - O-乙基-L-抗坏血酸,6 - O-棕榈酰-L-抗坏血酸和6- O-硬脂酰基-L-抗坏血酸可以在聚乙二醇300存在下有效地稳定II型拟除虫菊酯。三种抗坏血酸衍生物和聚乙二醇300的混合物被证明是多残留农药分析的有效分析物保护剂。此外,我们设计和评估了分析物保护剂化合物的新组合,而无需使用聚乙二醇或麻烦的亲水性化合物。因此,我们得到了一组10中期和长链饱和脂肪酸作为适合于丙酮/有效分析保护Ñ-己烷溶液,不会引起II型拟除虫菊酯的峰不稳定性。这些分析物保护剂在耐用性和可靠的定量方面,将可用于通过气相色谱-质谱法进行多残留农药分析。