發(fā)布時(shí)間：2018-10-31 11:45

【摘要】：以96批梔子不同炮制品為研究對(duì)象,高效液相色譜測(cè)定梔子苷含量為參考值,利用近紅外光譜儀積分球漫反射測(cè)定其光譜圖,建模波段取8 660~7 500,6 650~5 600和4 900~4 000cm~(-1),以標(biāo)準(zhǔn)正態(tài)變換(SNV)和二階導(dǎo)數(shù)法(2nd derivative)為預(yù)處理方法,主成分?jǐn)?shù)為8,采用偏最小二乘法(PLS)對(duì)83批梔子樣品建立梔子苷的定量校正模型,最終以13批梔子不同炮制品對(duì)模型進(jìn)行驗(yàn)證。結(jié)果,定量模型的內(nèi)部交叉驗(yàn)證決定系數(shù)(R2)為0.992 85,校正均方差(RMSEC)為0.240,預(yù)測(cè)均方差(RMSEP)為0.254,內(nèi)部交叉驗(yàn)證均方差(RMSECV)為0.386 91,RMSEP/RMSEC=1.06。模型驗(yàn)證得到的相對(duì)分析誤差(RPD)為8.81,絕對(duì)偏差范圍-0.39%~0.23%,說(shuō)明模型預(yù)測(cè)性較好。通過(guò)相關(guān)系數(shù)法,優(yōu)選樣品裝樣量、掃描次數(shù)、重復(fù)次數(shù)、分辨率實(shí)驗(yàn)條件;并由近紅外一階導(dǎo)和二階導(dǎo)圖,除去溫濕度和樣品水分影響波段,結(jié)合梔子苷對(duì)照品近紅外光譜圖,確定建模波段。首次利用NIRS法建立梔子不同炮制品梔子苷定量校正模型,方法簡(jiǎn)單快速,模型穩(wěn)定可靠、準(zhǔn)確性高,可同時(shí)應(yīng)用于不同炮制品梔子中梔子苷含量的預(yù)測(cè)。
[Abstract]:96 batches of Gardenia jasminoides (Gardenia jasminoides) processed with different processed products were used as the study object, the content of Gardenia was determined by HPLC as reference value, and the spectrogram was measured by diffuse reflectance of the integrated sphere of near infrared spectrometer. The modeling wave band was 8 660,500,500,650,50,600 and 49004000cm ~ (-1), respectively. Using standard normal transformation (SNV) and second derivative method (2nd derivative) as the pretreatment method, the main component was 8. The quantitative calibration model of gardenia was established by partial least square method (PLS) for 83 lots of gardenia samples. Finally, 13 batches of different processing products of Gardenia jasminoides were used to verify the model. The results showed that the internal cross validation determination coefficient (R2) of the quantitative model was 0.992 85, the corrected mean square error (RMSEC) was 0.240, the predicted mean square error (RMSEP) was 0.254, and the internal cross-validation mean square error (RMSECV) was 0.386 91rms EPP / RMSECC 1.06. The relative analysis error (RPD) obtained from the model verification is 8.81, and the absolute deviation range is -0.39 and 0.23, which indicates that the model is predictable. Through the correlation coefficient method, the sample loading quantity, scanning times, repetition times and resolution experimental conditions were optimized. The first and second order map of near infrared was used to remove the temperature and humidity and the influence band of sample moisture, and the modeling band was determined by combining with the near infrared spectrum of the reference substance of geniposide. For the first time, the NIRS method was used to establish a quantitative calibration model of gardenia in different processed products. The method was simple, rapid, stable, reliable and accurate, and could be used to predict the content of gardeniposide in different processed Gardenia jasminoides simultaneously.
【作者單位】： 廣東藥科大學(xué)中藥學(xué)院;國(guó)家中醫(yī)藥管理局中藥數(shù)字化質(zhì)量評(píng)價(jià)技術(shù)重點(diǎn)研究室;廣東高校中藥質(zhì)量工程技術(shù)研究中心;廣東省藥品檢驗(yàn)所;
【基金】：全國(guó)中藥炮制技術(shù)規(guī)范研究中醫(yī)藥行業(yè)科研專(zhuān)項(xiàng)(201207004-7)資助
【分類(lèi)號(hào)】：O657;R286.0

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