光谱学与光谱分析
光譜學與光譜分析
광보학여광보분석
SPECTROSCOPY AND SPECTRAL ANALYSIS
2013年
12期
3226-3230
,共5页
刘桦%赵鑫%齐天%亓云鹏%范国荣
劉樺%趙鑫%齊天%亓雲鵬%範國榮
류화%조흠%제천%기운붕%범국영
人参皂苷%近红外%大孔树脂%高效液相色谱
人參皂苷%近紅外%大孔樹脂%高效液相色譜
인삼조감%근홍외%대공수지%고효액상색보
Ginsenoside%Near-infrared%Macroporous resin%High performance liquid chromatography
利用近红外(NIR)光谱技术研究并建立可在线监测人参叶皂苷类成分的大孔树脂分离纯化工艺的方法。建立人参皂苷Rg1,Re和Rb1的高效液相色谱(HPLC)含量测定方法,收集人参叶提取物的40%乙醇大孔树脂洗脱液,采集其近红外光谱信息,并用已建立的 HPLC法测定其中人参皂苷Rg1,Re和Rb1的含量,结合偏最小二乘法(PLS )建立上述三种成分及人参总皂苷的定量分析模型。建模过程中,以决定系数(R2),交叉验证均方根误差(RMSECV)为指标,确定用于建模的最优近红外波段和光谱预处理方法,结果表明人参皂苷Rg1,Re ,Rb1及人参总皂苷模型的最佳建模波段均为12000.8~7499.8 cm -1, R2分别为0.9887,0.9603,0.9905和0.9701,RMSECV分别为0.0597,0.0722,0.00488和0.0755。将1个批次的人参叶提取物大孔树脂分离纯化工艺样品用于验证人参总皂苷定量分析模型的预测性能,总皂苷的NIR预测值和 HPLC测定值的相关系数为0.9928,平均预测回收率为100.52%,表明所建的模型预测效果良好。该法快速、简便、准确,可用于生产工艺过程中人参总皂苷的含量测定和质量控制。
利用近紅外(NIR)光譜技術研究併建立可在線鑑測人參葉皂苷類成分的大孔樹脂分離純化工藝的方法。建立人參皂苷Rg1,Re和Rb1的高效液相色譜(HPLC)含量測定方法,收集人參葉提取物的40%乙醇大孔樹脂洗脫液,採集其近紅外光譜信息,併用已建立的 HPLC法測定其中人參皂苷Rg1,Re和Rb1的含量,結閤偏最小二乘法(PLS )建立上述三種成分及人參總皂苷的定量分析模型。建模過程中,以決定繫數(R2),交扠驗證均方根誤差(RMSECV)為指標,確定用于建模的最優近紅外波段和光譜預處理方法,結果錶明人參皂苷Rg1,Re ,Rb1及人參總皂苷模型的最佳建模波段均為12000.8~7499.8 cm -1, R2分彆為0.9887,0.9603,0.9905和0.9701,RMSECV分彆為0.0597,0.0722,0.00488和0.0755。將1箇批次的人參葉提取物大孔樹脂分離純化工藝樣品用于驗證人參總皂苷定量分析模型的預測性能,總皂苷的NIR預測值和 HPLC測定值的相關繫數為0.9928,平均預測迴收率為100.52%,錶明所建的模型預測效果良好。該法快速、簡便、準確,可用于生產工藝過程中人參總皂苷的含量測定和質量控製。
이용근홍외(NIR)광보기술연구병건립가재선감측인삼협조감류성분적대공수지분리순화공예적방법。건립인삼조감Rg1,Re화Rb1적고효액상색보(HPLC)함량측정방법,수집인삼협제취물적40%을순대공수지세탈액,채집기근홍외광보신식,병용이건립적 HPLC법측정기중인삼조감Rg1,Re화Rb1적함량,결합편최소이승법(PLS )건립상술삼충성분급인삼총조감적정량분석모형。건모과정중,이결정계수(R2),교차험증균방근오차(RMSECV)위지표,학정용우건모적최우근홍외파단화광보예처리방법,결과표명인삼조감Rg1,Re ,Rb1급인삼총조감모형적최가건모파단균위12000.8~7499.8 cm -1, R2분별위0.9887,0.9603,0.9905화0.9701,RMSECV분별위0.0597,0.0722,0.00488화0.0755。장1개비차적인삼협제취물대공수지분리순화공예양품용우험증인삼총조감정량분석모형적예측성능,총조감적NIR예측치화 HPLC측정치적상관계수위0.9928,평균예측회수솔위100.52%,표명소건적모형예측효과량호。해법쾌속、간편、준학,가용우생산공예과정중인삼총조감적함량측정화질량공제。
A method was developed for online monitoring of the constituents of ginsenoside of Folium Ginseng in the column sep-aration and purification process using near-infrared (NIR) spectroscopy technology .Determination method of ginsenoside Rg1 , Re and Rb1 was developed by high performance liquid chromatography (HPLC) .After collecting 40%-ethanol eluant ,their NIR spectra were detected and the contents of Rg1 ,Re and Rb1 were determined by the above HPLC method .The quantitative analy-sis models of the above three compounds and the total ginsenosides were established using partial least squares (PLS) .During modeling ,coefficient of determination (R2 ) and root mean square errors of cross-validation (RMSECV) were regarded as the in-dexes to select optimal wave numbers and preprocessing methods .The optimal wave numbers of ginsenoside Rg1 ,Re ,Rb1 and total ginsenosides were all in the range of 12 000.8~7 499.8 cm -1 ;R2 were 0.988 7 ,0.960 3 ,0.990 5 and 0.970 1 ,respec-tively ;RMSECV were 0.059 7 ,0.072 2 ,0.004 88 and 0.075 5 ,respectively .A lot of samples ,collected during the column separation and purification process of Folium Ginseng extract ,were used to validate the predicttion effect of quantitative analysis model of total ginsenosides .As a result ,the correlation coefficient of NIR predicted value and HPLC value of total ginsenosides was 0.992 8 and the mean prediction recovery was 100.52% ,which indicated that the prediction effect of the developed model was satisfactory .This method was proved to be fast ,convenient and precise .It can be used for assaying and quality control of total ginsenosides in manufacture .