核磁共振碳谱法同时测定多种低温保护剂的浓度  

Simultaneous determination of concentrations of multiple cryoprotective agents by Carbon-13 nuclear magnetic resonance spectroscopy

作　　者：虞效益[1,2] 徐美娟 陈光明[1,2,3] 李威[1] 

机构地区：[1]浙江大学宁波理工学院,宁波315100 [2]浙江省制冷与低温技术重点实验室,杭州310027 [3]浙江大学制冷与低温研究所,杭州310027

出　　处：《低温工程》2018年第1期57-61,共5页Cryogenics

基　　金：国家自然科学基金(51406180);宁波市自然科学基金(2016A610214);浙江省制冷与低温技术重点实验室开放基金(2016007AA)

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)。A carbon-13 nuclear magnetic resonance spectroscopic （13C-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. 13C-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 δ20.70 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-propane- diol, respectively） and limit of quantitation （0.05 wt% , 0.04 wt% , 0.04 wt% and 0.04 wt% for glycer- ol, DMSO, EG and 1,2-propanediol, respectively）. This method was used to quantify five prepared sam- ples with the eoncentration raging from 0. 1 wt% to 0.5 wt% , and the resulting mean relative errors be- tween 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.

关 键 词：核磁共振 甘油 二甲亚砜 乙二醇 丙二醇 低温保护剂 

分 类 号：R318.52[医药卫生—生物医学工程]