【摘要】 建立了核磁共振碳谱法(13C-NMR)同时测定低温保护剂甘油、二甲亚砜、乙二醇和1,2-丙二醇浓度的方法。以重水-水为溶剂,2,2-二甲基-2-硅戊基-5-磺酸钠(DSS)为内参,用Bruker AVANCE III 600 MHz核磁共振波谱仪在脉冲序列zgig30,脉冲间隔2 s,扫描次数6 000,采样温度298K,谱宽设定126×10-6,采样时间1 s的条件下采集样品的碳谱。以化学位移分别在δ74.88、δ41.40、δ65.30和δ20.70的单峰作为甘油、二甲亚砜、乙二醇和1,2-丙二醇的定量峰。方法学考察结果表明,在给定浓度范围内,4种低温保护剂均呈现良好的线性关系(R2>0.997 8),精密度RSD<4.10%,重复性RSD<4.03%,检出限和定量限分别为0.02 wt%和0.05 wt%(甘油)、0.01 wt%和0.04 wt%(二甲亚砜)、0.01 wt%和0.04 wt%(乙二醇)、0.01 wt%和0.04 wt%(1,2-丙二醇)。采用本方法对浓度范围0.1 wt%—0.5 wt%的5份样品进行测试,实测值与理论值的平均相对偏差分别为4.57%(甘油)、1.57%(二甲亚砜)、6.13%(乙二醇)和2.40%(1,2-丙二醇)。更多还原

【Abstract】 A carbon-13 nuclear magnetic resonance spectroscopic(13 C-NMR) method was established for the simultaneous quantitation of glycerol,dimethyl sulfoxide(DMSO),ethylene glycol(EG) and 1,2-propanediol. Deuterium oxide-water was selected as solvent,and 2,2-dimethyl-2-silapentane-5-sulfonate(DSS) was used as the internal reference.13 C-NMR spectra were obtained with a Bruker AVANCE III 600 MHz spectrometer at the following conditions: pulse sequence zgig30,pulse width 2 s,scan number 6 000,temperature 298 K,spectra width 126 ppm,and acquisition time 1 s. The integration of signals at chemical shifts of δ 74. 88 for glycerol,δ 41. 40 for DMSO,δ 65. 30 for EG,and δ 20. 70 for 1,2-propanediol were chosen for quantification,respectively. Method validation was performed in the given concentration rangesin terms of linearity(R2> 0. 997 8),precision(RSD < 4. 10%),repeatability(RSD < 4. 03%),limit of detection(0. 02 wt%,0. 01 wt%,0. 01 wt% and 0. 01 wt% for glycerol,DMSO,EG and 1,2-propanediol,respectively) and limit of quantitation(0. 05 wt%,0. 04 wt%,0. 04 wt% and 0. 04 wt% for glycerol,DMSO,EG and 1,2-propanediol,respectively). This method was used to quantify five prepared samples with the concentration raging from 0. 1 wt% to 0. 5 wt%,and the resulting mean relative errors between the measured and theoretical values were 4. 57% for glycerol,1. 57% for DMSO,6. 13% for EG,and 2. 40% for 1,2-propanediol,respectively.更多还原