离子色谱法测定工艺过程中菊粉含量  

Determination of Inulin in Production Process by Ion Chromatography

作　　者：贾鹏禹[1] 孙蕊[1] 项洪涛[2] 赵琪 郑殿峰[1] JIA Peng-yu;SUN Rui;XIANG Hong-tao;ZHAO Qi;ZHENG Dian-feng(Heilongfiang Bayi Agricultural University,Daqing 163319,China;Crop Tillage and Cultivation Institute,Heilongjiang Academy of Agricultural Sciences,Harbin 150086,China;Qiqihaer Entry-Exit Inspection and Quarantine Bureau,Qiqihaer 161006,China)

机构地区：[1]黑龙江八一农垦大学,黑龙江大庆163319 [2]黑龙江省农业科学院耕作栽培研究所,黑龙江哈尔滨150086 [3]齐齐哈尔市出入境检验检疫局,黑龙江齐齐哈尔161006

出　　处：《药物生物技术》2018年第3期237-241,共5页Pharmaceutical Biotechnology

基　　金：国家自然科学基金项目(No.31571613;No.31271652);黑龙江八一农垦大学‘校内培育课题资助计划’项目(No.XZR2015-15);黑龙江省普通本科高等学校青年创新人才培养计划项目

摘　　要：为检测工业级菊粉生产中不同工艺过程中的菊粉含量及鉴定问题产品真伪,文章研究建立了菊粉含量的离子色谱测定方法及真伪鉴别方法。采用Dionex ICS5000+离子色谱仪,样品组分分离采用Carbo Pac PA2003 mm×250 mm色谱柱,配备同系保护柱Carbo Pac PA200 3 mm×50 mm,柱温30℃,体积流量0.40 m L/min,流动相采用梯度洗脱模式,流动相A(Na OH)在20~25 min内由6 mmol/L线性增至100 mmol/L并保持至50 min,流动相B(Na AC)在25~35 min内由0 mmol/L线性增至100 mmol/L并保持至50 min,检测器采用脉冲积分安培检测器,电极Au,参比电极Ag/Ag Cl,检测器电位波形为糖四电位波形,进样体积10μL,方法所用对照品采用Sepax Zenix SEC150+SEC100尺寸排阻制备色谱柱对菊粉成品进行纯化制备,纯化物采用傅里叶变换红外光谱进行结构表征,并采用shodex KS802配位体交换色谱柱进行纯度分析。结果表明采用尺寸排阻制备色谱纯化菊粉对照品具有可行性,所得菊粉对照品纯度为99.3%,满足未知样品定量需求,离子色谱分析得出菊粉线性方程为y=4.126x+1.391(R2=0.997 8),线性范围在0.10~5.00μg/m L之间,方法检测限为10.34 ng/m L,采用离子色谱法对问题样品进行真伪鉴别较尺寸排阻色谱具有更高的分离选择性。采用所建方法简单灵敏,能够有效地指导菊粉生产及鉴定产品真伪。In order to determine inulin in different processes of industrial production and to authenticate the authenticity of the problem product,in this paper,an analytical method for the determination of inulin in production process and its authenticity method were developed by using ion chromatography. The method was carried out on a Dionex ICS 5 000＋ion chromatography. The separation of sample was performed on a Carbo Pac PA200 column（ 3 mm × 250 mm） coupled with guard column by gradient elution using Na OHNa Ac as the mobile phase. The column temperature was set at 30 ° C,and the flow rate was 0. 40 m L/min. The mobile phase A（ Na OH） increased linearly in 20 ~ 25 min from 6 ~ 100 mmol/L and maintained to 50 min. The mobile phase B（ Na AC） increased linearly in 25 ~ 35 min from 0 ~ 100 mmol/L and maintained to 50 min. The PAD detector was gold electrode（ Au） at sugar four wave form potential and the reference electrode was Ag/Ag Cl. The injection volume was 10 μL. The reference substance of method was purified by size exclusion chromatography with Sepax Zenix SEC150 ＋ SEC100 column and inulin product,and characterized its structure by fourier transform infrared spectroscopy. Then the ligand exchange chromatography was used for purity analysis of reference substance with a Shodex KS802 column. The results showed that the size exclusion chromatography was feasible for the purification of inulin reference substance,and the purity of the inulin reference substance was 99. 3%,which could meet the quantitative requirement of unknown samples. The calibration curves developed for inulin were y = 4. 126 x ＋ 1. 391（ R2= 0. 997 8）,and had a good linear relationship within the concentration range of 0. 10 ~ 5. 00 μg/m L. The limit of detection of method was 10. 34 ng/m L.The identification of the problem sample by ion chromatography had a higher separation selectivity than the size exclusion chromatography. This method was simple and sensitive for directing the production of inulin effectively and a

关 键 词：离子色谱 脉冲积分安培检测 尺寸排阻色谱 工艺过程 菊粉 含量 真伪鉴别 

分 类 号：O657.7[理学—分析化学]