姜黄丸水分含量测定近红外定量模型的建立

目的: 运用近红外光谱(NIR)技术对姜黄丸水分进行快速测定。方法: 采集不同批次姜黄丸样品的近红外光谱图,结合OPUS软件进行预处理,在7 552.3~6 707.5 cm^-1,6 699.8~5 538.8 cm^-1,5 515.7~4 204.3 cm^-1谱段内,选择8个主成分,采用偏最小二乘法(PLS)建立姜黄丸水分近红外定量模型。结果: 所建模型相关系数(R²)为0.998 6,交互验证均方根偏差(RMSECV)为0.233,仪器精密度及样品重复性良好,所建模型可以准确测出姜黄丸水分含量。结论: 该方法具有快速、准确、简便的特点,可以用于大批量姜黄丸水分含量的快速在线检测。     

近红外漫反射光谱法测定头孢氨苄胶囊的含量

目的:应用近红外漫反射技术和化学计量学的方法对头孢氨苄胶囊进行定量分析.方法:通过偏最小二乘法建立数学模型,对预测集进行预测,并对实际样品的含量进行分析测定.结果:25个样品经内部交叉验证建立预测模型,内部交叉验证的均方差为0.40,确定系数R2=1.00.用15个样品进行外部验证,外部验证的均方差为0.59,确定系数R2=0.999.预测值与真值的确定系数为0.9995.预测值的平均回收率为100.4%(RSD为0.50%,n=15).方法精密度RSD为0.85%(n=7).结论:建立的预测模型对头孢氨苄胶囊进行含量测定是可行和有效的,样品不需预处理,分析快速、简便、环保,结果准确.     

近红外光谱技术在元胡止痛散定量分析中的初步应用研究

目的为元胡止痛散建立一种快速有效的定量分析方法,并为将近红外光谱分析技术应用于中药的定量分析提供指导。方法按处方配制25个模拟样本,随机挑选18个组成训练集,另外7个组成预示集,采集各样本的近红外光谱数据,用BP神经网络和PIS法对数据进行处理,并实际分析了三批样品。结果模拟样本中,对于元胡,采用BP网络和PLS法,平均相对预示误差分别为1．5％,2．5％,对于白芷,平均相对预示误差分另为2．9％,4．4％,对于实际样本,各组分标示量的百分含量都在95％～105％之间。结论近红外光谱结合BP神经网络或PLS应用于元胡止痛散的定量分析是可行和有效的。     

Process analytical technology: Non-destructive assessment of anastrozole entrapment within PLGA microparticles by near infrared spectroscopy and chemical imaging

The objective of this study was to evaluate near-infrared (NIR) spectroscopy and imaging as approaches to assess anastrozole entrapment within PLGA microparticles. By varying the polymer concentration, three batches containing the same amount of the drug were prepared. The spectral features that allow NIR drug quantitation were evaluated and compared with a best fit line algorithm. Actual entrapment efficiencies (EEF) determined via a destructive method were used for construction of calibration models using partial least square regression (PLS) or the algorithm. On the other hand, a chemical imaging system based on array detector technology was used to rapidly collect high contrast NIR images of the formulated microparticles. A quantitative measure of anastrozole entrapped was determined by calculating the percentage standard deviation of the distribution of pixel intensities in the PLS score images and histograms. Concerning conventional NIR analysis, both methods were equivalent for the prediction of EEF over the range of polymer levels studied. Correlation coefficients of more than 0.992 were obtained for either the calibration or prediction of EEF by the two methods; 0.392% and 0.374% were the standard errors of calibration and prediction (SEC and SEP) obtained for the prediction of EEF using the fit line, respectively, whereas the prediction of the EEF by the partial least square regression showed a SEC of 0.195% and SEP of 0.179%. As a result, the spectral best fit algorithm method compared favourably to the multivariate PLS method, but was easier to develop. In contrast, NIR spectral imaging was capable of clearly differentiating the three batches, both qualitatively and quantitatively. The percentage standard deviation increased progressively by increasing the ratio of drug-to-polymer concentrations. In conclusion, both NIR approaches were capable of accurate assessment of drug entrapment within microparticles. In addition, the NIR spectral imaging system provides a rapid approach for acquiring spatial and spectral information on microparticles.     

Sharp pH-sensitive amphiphilic polypeptide macrophotosensitizer for near infrared imaging-guided photodynamic therapy

Tumor environmental sensitive polypeptide integrated photosensitizer is a platform for imaging-guided photodynamic therapy (PDT). However, the photosensitizer leakage during blood circulation, poor accumulation in tumor tissue and inferior quantum yield of singlet oxygen are still challenges. Herein, NHS-active boron-dipyrromethene derivative with bromine substituted NHS-BODIPY-Br₂ was first synthesized, which possessed high singlet oxygen generation efficiency and near infrared (NIR) fluorescence, and then it was conjugated to a sharp pH (6.36) sensitive polypeptide to achieve a macrophotosensitizer for NIR imaging-guided PDT. In vitro study showed that the macrophotosensitizer nanoparticles exhibited good cellular uptake and ability to kill cancer cells. Once accumulating in the tumor tissues, the nanoparticles can be demicellized by tumor acidity to promote cellular uptake, which could enlarge fluorescence signal intensity and enhance in vivo PDT therapeutic effect upon NIR laser irradiation. It provides a strategy to design photosensitizer conjugated tumor acidity sensitive polypeptide for NIR imaging-guided photodynamic therapy.     

Determination of free amino acid content in Radix Pseudostellariae using near infrared (NIR) spectroscopy and different multivariate calibrations

Near infrared (NIR) spectroscopy combined with multivariate calibration was attempted to analyze free amino acid content of Radix Pseudostellariae. The original spectra of Pseudostellariae samples in wavelength range of 10000–4000 cm⁻¹ were acquired. Partial least squares (PLS), kernel PLS (k-PLS), back propagation neural network (BP-NN), and support vector regression (SVR) algorithms were performed comparatively to develop calibration models. Some parameters of the calibration models were optimized by cross-validation. The performance of BP-NN model was better than PLS, k-PLS, and SVR models. The root mean square error of prediction (RMSEP) and the correlation coefficient (R) of BP-NN model were 0.687 and 0.889 in prediction set respectively. Results showed that NIR spectroscopy combined with multivariate calibration has significant potential in quantitative analysis of free amino acid content in Radix Pseudostellariae.     

近红外漫反射光谱法测定红霉素肠溶片中红霉素A的含量

目的:应用近红外漫反射技术和化学计量学的方法对红霉素肠溶片中的红霉素 A 进行定量分析。方法:通过偏最小二乘法建立数学模型,对预测集进行预测,并对实际样品的含量进行测定。结果:40个校正集样品经内部交叉验证建立校正模型,内部交叉验证确定系数 R~2=99.86,内部交叉验证均方根误差(RMSECV)为0.50。对10个预测集样品进行外部验证,预测均方根误差(RMSEP)为0.493,预测值与真实值的相关系数达0.9995。预测值的平均回收率为100.11%(RSD=0.96%,n=10),方法精密度 RSD 为0.78%(n=8)。方法稳定性 RSD 为0.95%(n=7)。结论:本方法快速简便,结果准确,适用于药品快速检查和质量控制。     

近红外漫反射光谱法快速测定利福平含量

目的:应用近红外漫反射光谱结合偏最小二乘法(NIR-PLS)对利福平胶囊中利福平(RFP)含量进行测定。方法:采用偏最小二乘法(PLS)建立利福平胶囊中利福平含量的相关模型,并用所建立的模型对预测集样品中利福平含量进行预测。结果:所建定量分析模型回归系数r=0.9525。交互验证均方根误差(RMSECV)为0.0073。预测均方根误差(RMSEP)为0.0077。结论:该方法精确度高,且具有方便快捷、非破坏、无污染、成本低等优点,为药物非破坏性分析提供了一种快捷方法。     

近红外光谱法测定不同厂家天麻胶囊中的水分

目的应用近红外光谱技术建立天麻胶囊中水分定量快速测定的检测方法。方法通过对天麻胶囊的近红外光谱应用OPUS软件进行分析处理,建立水分定量测定模块,验证样品的数据基本符合。结果该方法能准确、快速测定天麻胶囊的水分,相对误差小于3%。结论该方法简便,快速,准确,重现性好,且不破坏样品,能应用于药品监督工作中对药品中水分的快速检测。     

消旋山莨菪碱非铝塑包装片剂近红外鉴别模型的初探

目的采用近红外漫反射光谱分析技术和模式识别技术建立消旋山莨菪碱非铝塑包装片剂定性分析模型用于该品种的鉴别。方法以8个生产厂家的消旋山莨菪碱为分析对象,采集近红外漫反射光谱,通过导数化和矢量归一化进行预处理,应用欧氏距离方法建立消旋山莨菪碱近红外鉴别数学模型。结果消旋山莨菪碱的定性分析模型的条件参数为：谱段为5 400-7 000 cm-1,光谱预处理方法为＂一阶导数法＋归一化＂,模型的阈值为0.603。并对模型进行了验证,能满足应用的要求。结论试验结果表明应用近红外光谱技术建立消旋山莨菪碱的定性分析模型是可行的,同时为模型更新提供了一个参考的方法。     

护肝片的近红外光谱鉴别研究

目的 运用近红外光谱,建立鉴别不同厂家生产的护肝片的定性分析模型.方法 采集样品近红外漫反射光谱,使用一阶导数和二阶导数加矢量归一化预处理后,分别建立了聚类分析模型和定性分析模型.结果 两种模型均能准确鉴别护肝片真伪.结论 该方法简便、快速、准确,可以在药品检测车中使用.     

利用NIR技术建立异烟肼片一致性比对模型的研究

目的应用近红外漫反射技术建立异烟肼片一致性检验模型快检方法。方法收集异烟肼片的近红外漫反射光谱,运用OPUS软件建立一致性检验模型,采用三台仪器对模型进行交叉验证,并用其它厂家生产的异烟肼片进行验证。结果模型通过仪器交叉验证,也能区分出其它厂生产的异烟肼,利用该一致性检验模型能无损伤、快速、准确地判断异烟肼片的真伪。结论该方法建立的模型操作简单、快速有效,能作为异烟肼片真伪鉴别的快速筛选方法。     

药物辅料中有毒掺杂物的拉曼/近红外光谱法检测灵敏度评价

目的 建立常用药物辅料(甘油)中有毒掺杂物(二甘醇)的快速检测方法。 方法 利用拉曼/近红外光谱法结合移动窗口相关系数法评价有毒掺杂物的检测灵敏度。 结果 拉曼光谱下获得的检测灵敏度优于近红外光谱,同时移动窗口法可进一步提高检测灵敏度。 结论 拉曼光谱法有望成为现场快速检测药物辅料中掺杂有毒物质的有效方法。     

Terahertz pulsed imaging and near infrared imaging to monitor the coating process of pharmaceutical tablets

Terahertz pulsed imaging (TPI) and near infrared (NIR) imaging were used to non-destructively monitor the coating process of film-coated tablets. Samples that were taken from a pan coater at different time points were analyzed by both methods. TPI provided coating thickness maps over the whole surface of the tablets, determining the thickness of the coating at each point of the sample surface in μm, this way also giving information about the coating uniformity. The growth of the coating during the coating process was shown. NIR imaging did not provide direct thickness values, but by different absorbance values, inter- and intra-tablet differences were shown. Thus, coating thickness information was also obtained in a way that different tablets could be compared. The growth of the coating layer during the process was shown as well. Both methods provided comparable results; and they were able to detect small defects in the coating. With TPI, the whole tablet surface could be scanned; with NIR imaging information about the tablet ends at the center-band was not obtained due to the strong curvature. NIR imaging proved to be better at thinner coating layers and had a higher spatial resolution whereas TPI had the clear advantage that it provided direct thickness values.     

不同产地大黄药材的近红外漫反射光谱法鉴别

目的:建立用近红外漫反射光谱鉴别不同产地大黄药材的新方法。方法:采集不同产地的大黄药材及其伪品的近红外漫反射光谱,分别用OPUS软件自带的聚类分析组件与第二军医大学药学院研发的近红外光谱-褶合变换-信息可视化-相似系数分析软件对其进行鉴别。结果:聚类分析的结果不甚理想,褶合变换分析得到正品与伪品大黄的相似系数<0.68,而正品大黄药材之间的相似系数均>0.81,同产地的药材之间的相似系数均>0.92。结论:近红外光谱法简便、快速,结合褶合变换分析得到的相似系数能够准确鉴别正品、伪品以及不同产地的大黄药材,所得分析结果与经典的形态分类学鉴别方法一致。     

偏最小二乘法用于近红外漫反射光谱快速测定异福片

目的:采用近红外光谱技术,建立一种快速测定异福片中利福平和异烟肼含量的方法。方法:将光谱分别进行卷积平滑、一阶导数、二阶导数预处理,应用偏最小二乘法(PLS)建立定量分析模型,以校正集的交互验证均方根误差(RMSECV)及相关系数(r)为优化参数,选择最佳预处理方法和波长范围。通过留一交互验证法,以预测残差平方和(PRESS)为优化参数,选择最适主因子数。结果:校正集样品利福平和异烟肼的 r 分别为0.9940和0.9910,RMSECV 分别为0.00764和0.00445。对预测集样品利福平和异烟肼的预测均方根误差(RMSEP)分别为0.00397和0.00383;平均加样回收率分别为100.88%和100.87%;重复性试验 RSD 分别为0.672%和1.08%。结论:结果表明该方法预测精度高,且具有方便快捷、非破坏、无污染、可在线检测、重复性好等优点,可作为异福片原位质量检测和在线质量监控的方法予以推广。     

近红外光谱技术在食品安全方面的应用进展

简要介绍了近红外光谱技术的发展历程,产生及测定过程,现代近红外光谱技术的特点以及近红外光谱技术在粮食、食用油、肉类、乳制品、果蔬、茶叶等食品安全方面的应用和检测中的局限性以及存在问题。     

硫酸羟氯喹颗粒水分近红外光谱在线定量模型的建立

目的 为实时检测硫酸羟氯喹颗粒在流化床干燥过程中的水分含量变化,建立颗粒水分的在线近红外光谱定量模型.方法 物料颗粒在流化床的干燥过程中,实时取样并用水分测定仪测量颗粒水分,采用多元散射校正(multiplicative signal correction,MSC)、一阶导数和Karl Norris平滑的光谱预处理方法...     

近红外快速鉴别保健品中非法添加盐酸丁二胍的方法

目的 利用近红外特征谱段相关系数法建立快速鉴别保健品中非法添加盐酸丁二胍的方法.方法 以盐酸丁二胍对照品的近红外光谱图为参照光谱,选择特征谱段,根据已知样本的近红外光谱与参照光谱的相关系数、盐酸丁二胍的有效剂量,确定阈值,建立检测模型.结果 选定7294～7402cm-1,5354～5432cm-1波数为特征谱段,设定阈值r=80%,用10批含盐酸丁二胍的样品进行验证,相关系数高于阈值的有10批,占样品总量的100%;用7批不含盐酸丁二胍的降糖类样品进行验证,相关系数低于阈值的有6批,占样品总量的85.71%.结论 该方法具有较好的预测能力,可用于保健品中非法添加盐酸丁二胍的快速检测.     

近红外光谱快速评价丹参基地药材

目的：采用近红外（NIR）光谱和相似度匹配值方法对丹参药材整体质量进行无损快速评价。方法：以62批丹参药材为具体研究对象，采集其NIR漫反射光谱，以其中10批基地药材作为标准样品集，建立相似度匹配模型，并将其用于计算其余52批药材的相似度匹配值。结果：相似度匹配值能反映各批次丹参药材与基地丹参药材的质量差别，并能准确区分基地药材和其他产地的药材。结论：该法能够快速、有效地评价丹参药材整体质量，为中药材的整体质量评价提供了一种新手段。