近红外漫反射光纤光谱结合偏最小二乘法快速测定黑果小檗皮中盐酸小檗碱含量

目的应用近红外漫反射光纤光谱结合偏最小二乘法(NIR-PLSR)对黑果小檗皮中盐酸小檗碱进行快速定量分析。方法建立NIR-PLSR数学模型对黑果小檗皮中盐酸小檗碱进行快速定量分析。结果黑果小檗皮中盐酸小檗碱的内部交叉验证均方差(RMSECV)为0.810 2,内部交叉验证决定系数为0.987 1,预测平均回收率为101.4%,统计学检验表明NIR预测值与标准方法测定值之间的差异无统计学意义。结论利用NIR-PLSR对黑果小檗进行定量分析可行。     

近红外漫反射光纤光谱法快速鉴别新疆黑果小檗皮

目的：探讨近红外漫反射光纤光谱技术结合主成分分析和聚类分析对黑果小檗皮产地及真伪进行鉴别。方法建立主成分分析（PCA）及聚类分析模型来鉴别黑果小檗皮。结果主成分分析及聚类分析可将收集到的39份黑果小檗皮样本分为3大产区,所建立的定性鉴别模型对其余14份预测集样本进行鉴别,分析结果与实际所属基本一致。表明利用近红外光谱法对黑果小檗皮进行产地及真伪鉴别可行（P＜0．05）。结论该模型鉴定黑果小檗皮快速、准确可靠、测量重现性好、样品测量一般无需预处理且分析过程不破坏样品。     

新疆特色药材黑果小檗薄层鉴别方法研究

目的建立新疆特色药材黑果小檗的薄层鉴别系统。方法以盐酸药根碱、盐酸巴马汀、盐酸小檗碱为对照品,对黑果小檗药材进行薄层鉴别,并考察不同展开系统、不同点样量、不同薄层板、不同检视方式、不同温度、不同湿度对黑果小檗药材薄层色谱的影响。结果以盐酸药根碱、盐酸巴马汀、盐酸小檗碱为对照品,以甲苯-乙酸乙酯-甲醇-异丙醇-氨水(6∶3∶2∶1.5∶0.5)为展开系统,黑果小檗药材薄层鉴别特征明显,专属性强。结论该方法可行,重复性好,可作为黑果小檗药材的薄层鉴别方法。     

近红外漫反射光谱法无损快速测定头孢丙烯原料药中的水分

目的采用近红外漫反射光谱技术结合偏最小二乘回归建立了测定头孢丙烯原料药中水分的定量分析模型。方法以头孢丙烯原料药为研究对象,用近红外光纤探头采集其近红外漫反射光谱,用费休氏法测定实际水分含量,运用偏最小二乘回归建立近红外光谱特征值与实际水分含量之间的校正模型,进而对预测集样品进行分析。结果在水分含量0.7%～9.8%范围内,校正集样品经内部交叉检验和检验集检验,相关系数(r)为0.999 6,内部交叉验证均方差(RMSECV)和外部检验均方差(RMSEP)分为0.40和0.41。结论所建模型具有较好的预测能力,结果可靠,为头孢丙烯原料药的质量控制提供了一种快速简便的检测方法。     

近红外光谱法快速测定山橿药材中球松素含量

目的利用近红外光谱（NIR）技术建立一种山橿中球松素含量的快速分析方法。方法以HPLC分析值为参照,采用近红外漫反射光谱技术采集66份山橿样品的近红外漫反射光谱,结合偏最小二乘法（PLS）建立了球松素含量的定量分析模型。结果所建模型的相关系数（R2）、外部验证均方差（RMSEP）和内部交叉验证均方差（RMSECV）分别为0.992 31、0.076 5和0.450 0;验证集样品的NIR测得值与药典法测得值进行配对T检验,差异无统计学意义。结论本方法操作简便、无污染、结果准确可靠,可用于山橿中球松素含量的快速测定。     

AOTF近红外光谱技术快速测定茯苓中的水分

目的：采用AOTF近红外漫反射光谱仪,建立茯苓中水分的快速定量分析方法。方法：以空气为背景,采用漫反射方式、SNAP光谱采集软件,采集近红外光谱,光谱数据为比率模式下采集,利用偏最小二乘法（PLS）、交叉-验证法（cross-validation）及Unscrambler定量分析软件创建定量校正模型。结果：定量模型的外部验证相关系数和内部验证相关系数均能达到0.9950,通过模型外部验证,验证集相对偏差RSEP值为2.7%,验证集预测误差均方根RMSEP值为0.49,预测值和化验值的平均相对偏差为1.3%。结论：AOTF近红外漫反射光谱仪可达到对茯苓药材中水分含量快速准确测定的目的。     

民族药黑果小檗根的质量控制

目的:建立黑果小檗根的质量控制标准,为药用植物资源的开发利用提供科学依据。方法:薄层色谱法、水分测定法、灰分测定法及HPLC法。结果:以盐酸小檗碱和盐酸药根碱为对照品,确定了黑果小檗根药材的薄层色谱鉴别方法、检查项测定了黑果小檗根的水分、灰分、酸不溶性灰分;同时暂定其活性成分盐酸小檗碱含量不得少0.60%。结论:通过研究制定了黑果小檗根药材的质量控制标准。     

近红外光谱技术快速测定杞菊地黄丸的水分含量

目的应用近红外光谱技术建立一种杞菊地黄丸(浓缩丸)中水分含量的快速测定方法。方法以甲苯法测定的样品中水分的含量为真实值,运用近红外漫反射光谱技术采集96份杞菊地黄丸(浓缩丸)样品的近红外漫反射光谱,结合偏最小二乘法(PLS)建立水分含量的定量分析模型。结果所建水分校正模型的相关系数(R2)和内部交叉验证均方差(RMSECV)分别为0.988 09和0.0587;经外部验证,模型的预测相关系数(r2)和预测均方差(RMSEP)分别为0.9969和0.075 2。结论该方法操作简便,无污染,结果准确可靠,可用于杞菊地黄丸(浓缩丸)中水分含量的快速测定。     

黄柏中多种生物碱测定的NIR模型的建立

目的:建立黄柏中3个成分(木兰花碱、黄柏碱、小檗碱)测定的NIR模型。方法:以高效液相测定的黄柏生物碱含量值作为参照,运用近红外漫反射光谱采集49批不同产地样品的近红外漫反射光谱,采用偏最小二乘算法(PLS)建立校正模型,比较不同的预处理方法及不同的波段对建模的影响。结果:以MSC+2D2为预处理方法,建立的小檗碱、黄柏碱、木兰花碱模型交互验证均方根误差(RMSEC)分别为0.0453、0.0335、0.0396,相关系数(R2)分别为0.9995、0.9760、0.9306。结论:建立的NIR模型稳定准确可靠,适用于生产中快速在线检测。     

近红外光谱法快速分析注射用头孢曲松钠及其水分的含量

目的：利用近红外漫反射光谱（NIRDRS）分析技术和化学计量学方法对注射用头孢曲松钠及其水分进行无损、快速定量分析。方法：以全国不同企业生产的注射用头孢曲松钠为分析对象，用光纤测定近红外漫反射光谱，采用偏最小二乘法（PLS）算法建立模型。结果：注射用头孢曲松钠定量分析模型由60个样品经内部交叉验证建立，85个样品用于外部验证，浓度范围为72．1％～90．6％，相关系数为0．9712，交叉验证均方差（RMSECV）为1．21，外部验证均方差（RMSEP）为1．07。注射用头孢曲松钠水分定量分析模型由56个样品经内部交叉验证建立，62张光谱用于外部验证，浓度范围为2．8％～9．9％，相关系数为0．9930，RMSECV为0．271，RMSEP为0．294。结论：2个模型结合可以按药典要求对注射用头孢曲松钠含量进行快速预测，方法快速、简便，可用于药品的现场快速分析。     

Prediction of tablets disintegration times using near-infrared diffuse reflectance spectroscopy as a nondestructive method

The goals of this study are to user near-infrared reflectance (NIR) spectroscopy to measure the disintegration time of a series of tablets compacted at different compressional forces, calibrate NIR data vs. laboratory equipment data, develop a model equation, validate the model, and test the model's predictive ability. Seven theophylline tablet formulations of the same composition but with different disintegration time values (0.224, 1.141, 2.797, 5.492, 9.397, 16.8, and 30.092 min) were prepared along with five placebo tablet formulations with different disintegration times. Laboratory disintegration time was compared to near-infrared diffuse reflectance data. Linear regression, quadratic, cubic, and partial least square techniques were used to determine the relationship between disintegration time and near-infrared spectra. The results demonstrated that an increase in disintegration time produced an increase in near-infrared absorbance. Series of model equations, which depended on the mathematical technique used for regression, were developed from the calibration of disintegration time using laboratory equipment vs. the near-infrared diffuse reflectance for each formulation. The results of NIR disintegration time were similar to laboratory tests. The near-infrared diffuse reflectance spectroscopy method is an alternative nondestructive method for measurement of disintegration time of tablets.     

Moisture assay of an antifungal by near-infrared diffuse reflectance spectroscopy

Near-infrared (NIR) diffuse reflectance spectroscopy was employed in the method development and validation of a moisture assay for the novel antifungal caspofungin acetate. Spectra were obtained over the entire spectral region available (950-1650 nm) using an InGaAs photodiode array detector equipped with a diffuse reflectance probe. No sample pre-treatment was required and the analysis time was less than 1 min. Primary reference data were obtained using a Karl Fischer (KF) titration (coulometric, volumetric or both). The investigated range of water content was 2.6-9.9% (w/w) with a standard error of prediction (SEP) of 0.2%. The predictive capabilities of the partial least-squares (PLS) regression calibration model used in the moisture assay were verified using independent test sets. The NIR predicted values of the developed method were equivalent to the reference method sets and the prediction error was equivalent to the reference method error. These results reveal that the predictive model constructed by means of a PLS regression is valid, rugged and could be used to determine moisture levels on-line in caspofungin acetate drug substance.     

Prediction of drug dissolution from tablets using near-infrared diffuse reflectance spectroscopy as a nondestructive method

The goal of this study is to use near-infrared (NIR) reflectance spectroscopy to measure the percentage drug dissolution from a series of tablets compacted at different compressional forces, calibrate NIR data vs. laboratory equipment data, develop a model equation, validate the model, and test the model predictive ability. Seven theophylline tablet formulations of the same composition but with different dissolution profiles were prepared. Laboratory dissolution profiles were compared with NIR diffuse reflectance data. Linear regression, quadratic, cubic, and partial least-square techniques were used to determine the relationship between dissolution profiles data and NIR spectra. The results demonstrated that a decrease in the amount of drug dissolution produced an increase in NIR absorbance. A series of model equations, depending on the mathematical technique used for regression, were developed from the calibration of the percentage of drug dissolution by using laboratory equipment vs. the NIR diffuse reflectance for each formulation. The results of NIR dissolution data were similar to laboratory tests. The NIR diffuse reflectance spectroscopy method is an alternative, nondestructive method for measurement of drug dissolution from tablets.     

近红外漫反射光谱法测定盐酸布比卡因微球含量

目的：采用近红外漫反射光谱（NIRDRS）技术,建立一种快速测定微球主药含量的方法。方法：建立校正样品集与测试样品集,采集近红外光谱,运用偏最小二乘法建立数学模型,对测试集进行预测。结果：校正样品集的最佳主成分数为Rank=6,内部交叉验证均方差（RMSECV）=2．38,决定系数R^2=93．18。测试样品集的预测结果：预测均方差（RMSEP）=2．37,决定系数R^2=93．77,评估均方差（RMSEE）=3．37。结论：NIRDRS测定微球的含量结果可靠,该技术应用于微球制剂生产的在线监测、评价微球制剂的质量标准提供了坚实的理论依据。     

黑果小檗总黄酮含量测定及体外抗氧化活性研究

目的测定黑果小檗各部位中总黄酮含量并评价其体外抗氧化活性,为有效利用黑果小檗资源提供参考。方法采用紫外分光光度法测定黑果小檗中总黄酮的含量,并通过DPPH、羟自由基和氧自由基清除法评价黑果小檗提取物的抗氧化活性。结果黑果小檗果实中总黄酮含量较高;其次为茎皮及根皮;果实提取液的抗氧化活性较强,茎皮次之。结论黑果小檗提取物具有一定的抗氧化能力,本研究可为天然抗氧化剂的开发提供依据。