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Effects of Residual Silanol on Solid Phase Extraction of Organic Compounds to Octadecylsilyl Silica
Analytical Sciences ( IF 1.6 ) Pub Date : 2021-06-10 , DOI: 10.2116/analsci.20p314
Satoshi OHMURO 1 , Ryo ISHIZAKI 1 , Masashi TSUKAMOTO 1 , Shizuka NASU 1 , Takashi YASUI 1 , Kazutake TAKADA 1 , Akio YUCHI 1
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Batchwise equilibrium study was carried out on the retention of nonpolar and polar organic compounds to octadecylsilyl (ODS) silicas of different properties at atmospheric pressure. While nonpolar compounds were retained only by distribution on the ODS phase, polar compounds were retained by both distribution and Langmuir-type adsorption on residual silanol. Retention on ODS silica with more silanol proceeded at a higher rate than retention on ODS silica with less silanol and was reversible on this solid phase extraction time-scale. An increase in surface density of ODS decreased the distribution constant, due to a decrease in fraction of ODS functioning as an extracting medium and also decreased the saturated adsorption amount, due to reductions of the residual silanol and the functioning ODS. The ODS silica with the lowest ODS density showed a distribution constant 31 times higher and a saturated adsorption amount 27 times higher than the ODS silica with the highest ODS density. On the other hand, because the interaction between the organic part and the ODS group introduced at higher density is strengthened, the adsorption constant is increased by about 5 times compared to the low density ODS silica. The electronic effects of substituents to nitrogen- and oxygen-containing compounds on retention were discussed. In conclusion, ODS silica with an appreciable amount of residual silanol is superior for solid phase extraction.

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中文翻译:

残留硅烷醇对有机物固相萃取十八烷基硅石的影响

对大气压下不同性质的十八烷基甲硅烷基 (ODS) 二氧化硅对非极性和极性有机化合物的保留进行了分批平衡研究。非极性化合物仅通过分布在 ODS 相上而被保留,而极性化合物则通过分布和朗缪尔型吸附在残余硅烷醇上而被保留。在具有更多硅烷醇的 ODS 硅胶上的保留率高于在具有较少硅烷醇的 ODS 硅胶上的保留率,并且在该固相萃取时间尺度上是可逆的。ODS 表面密度的增加降低了分布常数,这是由于作为提取介质的 ODS 部分的减少,并且由于残留硅烷醇和功能性 ODS 的减少,也降低了饱和吸附量。ODS 密度最低的 ODS 二氧化硅的分布常数比 ODS 密度最高的 ODS 二氧化硅高 31 倍,饱和吸附量高 27 倍。另一方面,由于有机部分与以较高密度引入的 ODS 基团之间的相互作用得到加强,与低密度 ODS 二氧化硅相比,吸附常数增加了约 5 倍。讨论了含氮和含氧化合物的取代基对保留的电子效应。总之,具有可观量残留硅烷醇的 ODS 硅胶更适合固相萃取。由于有机部分与高密度引入的ODS基团之间的相互作用得到加强,与低密度ODS二氧化硅相比,吸附常数增加了约5倍。讨论了含氮和含氧化合物的取代基对保留的电子效应。总之,具有可观量残留硅烷醇的 ODS 硅胶更适合固相萃取。由于有机部分与高密度引入的ODS基团之间的相互作用得到加强,与低密度ODS二氧化硅相比,吸附常数增加了约5倍。讨论了含氮和含氧化合物的取代基对保留的电子效应。总之,具有可观量残留硅烷醇的 ODS 硅胶更适合固相萃取。

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更新日期:2021-06-09
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