Two polysaccharide-based chiral stationary phase columns were evaluated to improve the previous partial chiral peak separation to a baseline-resolved separation of the INGREZZA® drug substance and its diastereome...Two polysaccharide-based chiral stationary phase columns were evaluated to improve the previous partial chiral peak separation to a baseline-resolved separation of the INGREZZA® drug substance and its diastereomers. Moreover, the tailing factor (Tf) variation was studied to investigate chiral column degradation and regeneration and to optimize chiral column performance and efficiency.展开更多
目的建立电纺聚苯乙烯纳米纤维固相萃取-气相色谱质谱法测定复合膜袋中27种芳香胺的迁移量的方法。方法样品经活化的、由电纺纳米聚苯乙烯材料制作的固相萃取小柱上样后,使用叔丁基甲醚洗脱,采用程序升温进样口进样。采用气相色谱质谱法...目的建立电纺聚苯乙烯纳米纤维固相萃取-气相色谱质谱法测定复合膜袋中27种芳香胺的迁移量的方法。方法样品经活化的、由电纺纳米聚苯乙烯材料制作的固相萃取小柱上样后,使用叔丁基甲醚洗脱,采用程序升温进样口进样。采用气相色谱质谱法(gas chromatography mass spectrometry,GC-MS)测定复合膜袋中27种游离芳香胺在水基食物模拟物中的迁移量,选择离子内标法定量。结果电纺纳米聚苯乙烯材料对水基食品模拟物中的芳香胺具有很好的吸附分离能力,27种芳香胺的回收率为80.2%~110.4%,精密度在2.0%~6.9%之间,定量限达到0.01 mg/kg。结论电纺纳米材料比表面积大,且对芳香胺类物质有较好的吸附能力,在满足标准方法检出限的要求下大大降低了洗脱有机溶剂的使用量,该种材料在仪器分析中有较强的应用前景,且该方法准确、灵敏,适用于水基食物模拟物中的27种芳香胺含量的测定。展开更多
The interaction index c which was derived from the fundamental retention equationlogk’ =a + cC_B in reversed--phase high--performancc liquid chromatography (RP-HPLC) quan-titatively describes the difference in the in...The interaction index c which was derived from the fundamental retention equationlogk’ =a + cC_B in reversed--phase high--performancc liquid chromatography (RP-HPLC) quan-titatively describes the difference in the interaction between solute--strong. solvent andsolute--weak solvent; it has shown to be a constant for a specific solute even when columnsystems with different C18 packings are used. The theoretical basis for peak identificationby using interaction index has been proposed, which was based on the a,c values on stan-dard C18 column by utilizing linear a-a plots on column pairs and the linear relationship be-tween parameters a and c for the structural related compounds. Through the establishmentof parameters a,c data based on the standard C18 column for a certain type of compounds,the retention of thesc compounds on various C18 columns can be predicted. Typical exam-ples have been given to verify the correctness of this method.展开更多
Based on the fact that the first set of the linear relationship between z and lg/ ofstoichiometric displacement model for retention in reversed-phase liquid chromatography is separatelyproportional to contact surface ...Based on the fact that the first set of the linear relationship between z and lg/ ofstoichiometric displacement model for retention in reversed-phase liquid chromatography is separatelyproportional to contact surface area,a linear relationship between z and lg/ for both of polar and apolarsmall solute molecules was theoretically derived and experimentally tested.The j obtained,one of the secondset of the linear parameters,is a characterization parameter for organic solvent strength and the column phaseratio(?)is defined as the value of k’ when the partition coefficient of solute in two phases is unity.展开更多
文摘Two polysaccharide-based chiral stationary phase columns were evaluated to improve the previous partial chiral peak separation to a baseline-resolved separation of the INGREZZA® drug substance and its diastereomers. Moreover, the tailing factor (Tf) variation was studied to investigate chiral column degradation and regeneration and to optimize chiral column performance and efficiency.
文摘目的建立电纺聚苯乙烯纳米纤维固相萃取-气相色谱质谱法测定复合膜袋中27种芳香胺的迁移量的方法。方法样品经活化的、由电纺纳米聚苯乙烯材料制作的固相萃取小柱上样后,使用叔丁基甲醚洗脱,采用程序升温进样口进样。采用气相色谱质谱法(gas chromatography mass spectrometry,GC-MS)测定复合膜袋中27种游离芳香胺在水基食物模拟物中的迁移量,选择离子内标法定量。结果电纺纳米聚苯乙烯材料对水基食品模拟物中的芳香胺具有很好的吸附分离能力,27种芳香胺的回收率为80.2%~110.4%,精密度在2.0%~6.9%之间,定量限达到0.01 mg/kg。结论电纺纳米材料比表面积大,且对芳香胺类物质有较好的吸附能力,在满足标准方法检出限的要求下大大降低了洗脱有机溶剂的使用量,该种材料在仪器分析中有较强的应用前景,且该方法准确、灵敏,适用于水基食物模拟物中的27种芳香胺含量的测定。
文摘The interaction index c which was derived from the fundamental retention equationlogk’ =a + cC_B in reversed--phase high--performancc liquid chromatography (RP-HPLC) quan-titatively describes the difference in the interaction between solute--strong. solvent andsolute--weak solvent; it has shown to be a constant for a specific solute even when columnsystems with different C18 packings are used. The theoretical basis for peak identificationby using interaction index has been proposed, which was based on the a,c values on stan-dard C18 column by utilizing linear a-a plots on column pairs and the linear relationship be-tween parameters a and c for the structural related compounds. Through the establishmentof parameters a,c data based on the standard C18 column for a certain type of compounds,the retention of thesc compounds on various C18 columns can be predicted. Typical exam-ples have been given to verify the correctness of this method.
基金the National Natural Science Foundation of China
文摘Based on the fact that the first set of the linear relationship between z and lg/ ofstoichiometric displacement model for retention in reversed-phase liquid chromatography is separatelyproportional to contact surface area,a linear relationship between z and lg/ for both of polar and apolarsmall solute molecules was theoretically derived and experimentally tested.The j obtained,one of the secondset of the linear parameters,is a characterization parameter for organic solvent strength and the column phaseratio(?)is defined as the value of k’ when the partition coefficient of solute in two phases is unity.
