摘要
本文建立了针对10种寡糖,包括甘露糖醛酸(M)和古罗糖醛酸(G)的离子色谱串联三重四极杆质谱的分析方法.优化后的离子色谱条件:Thermo Scientific Dionex IonPac^(TM) AS19-4μm(2 mm×250 mm,Analytical),200 mmol·L^(-1)氢氧化钠-水为淋洗液,流速0.3 mL·min^(-1),柱温30℃,电导检测器后连外接泵,三通阀加0.25 mL·min^(-1)乙腈.采用ESI源,扫描方式为选择反应检测.结果表明,离子色谱对不同聚合度的甘露糖醛酸和古罗糖醛酸有很好的保留和分离效果,三重四极杆质谱相比传统检测手段具有优异的灵敏度和高选择性;稳定性良好,连续进样5针,RSD均小于6.08%;标曲线性关系良好,R^(2)≥0.9990;方法检出限0.34μg·L^(-1);加标回收率均≥90.2%,本方法可用于寡糖的定性及定量分析.
In this paper,an ion chromatography coupled with triple quadrupole mass spectrometry method was developed for 10 oligosaccharides,including mannuronic acid(M)and guluronic acid(G).Optimized ion chromatographic conditions:Thermo Scientific Dionex IonPac^(TM) AS19-4μm(2 mm×250 mm,Analytical),200 mmol·L^(-1)sodium hydroxide-water as eluent,flow rate0.3 L·min^(-1),column temperature 30℃,conductivity detector connected to the back External pump,add0.25 mL·min^(-1)acetonitrile.The ESI source was used,and the scanning method was selective reaction detection(SRM).The results show that:ion chromatography had good retention and separation effects on mannuronic acid and guluronic acid with different degrees of polymerization,triple quadrupole mass spectrometry has excellent sensitivity and high selectivity compared with traditional detection methods;continuous in 5 injections,the RSDs were all less than 6.08%.The calibration curve has a good linear relationship,R^(2)≥0.9990;the detection limit of the method is 0.34μg·L^(-1);the detection results are accurate,and the recovery of the low,middle and high levels of the standard is greater than or equal to 90.2,so this method can be used for the qualitative analysis of oligosaccharides and quantitative analysis.
作者
江竹莲
陈雪煜
王林
JIANG Zhulian;CHEN Xueyu;WANG Lin(Chia Tai Tianqing Pharmaceutical Group Co.,Ltd,Lianyungang,222006,China;Nanjing University of Chinese Medicine,Nanjing,210023,China)
出处
《环境化学》
CAS
CSCD
北大核心
2022年第4期1453-1456,共4页
Environmental Chemistry
关键词
寡糖
离子色谱-质谱联用
TSQ
Altis
oligosaccharide
ion chromatography coupled with triple quadrupole mass spectrometry
TSQ Altis