Spectral characteristics of the correlation between elemental arsenic and vegetation stress in the Yueliangbao gold mining.

Some soils in the Yueliangbao gold mining area have been contaminated by heavy metals, resulting in variations in vegetation. Hyperspectral remote sensing provides a new perspective for heavy metal inversion in vegetation. In this paper, we collected ground truth spectral data of three dominant vegetation species, Miscanthus floridulus, Equisetum ramosissimum and Eremochloa ciliaris, from contaminated and healthy non-mining areas of the Yueliangbao gold mining region, and determined their heavy metal contents. Firstly, we compared the spectral characteristics of vegetation in the mining and non-mining areas by removing the envelope and derivative transformation. Secondly, we extracted their characteristic identification bands using the Mahalanobis distance and PLS-DA method. Finally, we constructed the inverse model by selecting the vegetation index (such as the PRI, DCNI, MTCI, etc.) related to the characteristic band combined with the heavy metal content. Compared to previous studies, we found that the pollution level in the Yueliangbao gold mining area had greatly reduced, but arsenic metal pollution remained a serious issue. Miscanthus floridulus and Eremochloa ciliaris in the mining area exhibited obvious arsenic stress, with a large "red-edge blue shift" (9 and 6 nm). The extracted characteristic wavebands were around 550 and 680-740 nm wavelengths, and correlation analysis showed significant correlations between vegetation index and arsenic, allowing us to construct a prediction model for arsenic and realize the calculation of heavy metal content using vegetation spectra. This provides a methodological basis for monitoring vegetation pollution in other gold mining areas.

Chemo-metric assisted UV-spectrophotometric methods for simultaneous estimation of Darunavir ethanolate and Cobicistat in binary mixture and their tablet formulation.

Darunavir ethanolate (DRV) and Cobicistat (CBS) is a combination of antiretroviral drugs used for the treatment of human immunodeficiency virus (HIV) infections. Two Chemo-metric assisted UV-spectrophotometric methods were developed for simultaneous estimation of DRV and CBS in tablet dosage form, namely; partial least square (PLS) and Classical least square method (CLS). The proposed methods were successfully applied for simultaneous determination of DRV and CBS in a laboratory mixture and their tablet formulation to achieve maximum sensitivity and lowest error. The applied methods were validated as per ICH guidelines and found to be linear in the concentration range of 5-30µg/mL for DRV and 5-30µg/mL for CBS. The developed methods were statistically comared with reported UPLC method where no significant difference was found relating to both accuracy and precision. Thus, the proposed methods can be effectively utilized for the routine quality control assessment of these drugs in commercial tablet dosage form.

[Quality research of Puerariae Lobatae Radix from different habitats with UPLC fingerprint and determination of multi-component content].

To establish ultra performance liquid chromatography( UPLC) fingerprint of Puerariae Lobatae Radix from different habitats and simultaneously determine the contents of six isoflavonoids. The UPLC fingerprint analysis and content determination were performed on a Waters ACQUITY UPLC BEH C_(18)( 2. 1 mm×50 mm,1. 7 µm) chromatographic column,with acetonitrile-0. 05% formic acid as mobile phase for gradient elution. The detection wavelength was set at 250 nm; the flow rate was 0. 2 mL·min~(-1); the column temperature was 30 ℃ and the injection volume was 2 µL. Similarity evaluation system for chromatographic fingerprint of traditional Chinese medicine( TCM) was adopted; principal component analysis( PCA) and discriminant analysis by partial least square method( PLS-DA) in Simca-P software were used to identify the differential components in samples from three habitats. The similarity was over 0. 90 in 29 batches of samples,indicating good consistency of the samples. The samples were clustered into 3 categories by PCA and PLS-DA,and six differential components such as puerarin apioside,daidzin,and isoflavoues aglycone were found. The determination results of 6 isoflavones,including 3'-hydroxy puerarin,puerarin,3'-methoxy puerarin,puerarin apioside,daidzin,and isoflavoues aglycone,showed that the content of the same component and the fluctuation range between different components were all different among different habitats. The total content of 6 isoflavones from different regions was Anhui 11. 21% >Henan 10. 97% >Shannxi 9. 38%. The establishment of UPLC fingerprint combined with simultaneous determination of 6 active components provides a more comprehensive reference for quality control and quality evaluation of Puerariae Lobatae Radix.

Application Status of Near Infrared Spectroscopy Combined with Chemometrics in Analysis of Traditional Chinese Medicine / 中国实验方剂学杂志

In recent years, near-infrared spectroscopy has developed into an analytical technique widely used in various fields. Because of its advantages of fast, green and non-destructive, it plays an increasingly prominent role in the field of traditional Chinese medicine (TCM) analysis. However, due to the complexity and overlap of spectra, near-infrared spectroscopy needs to be combined with chemometrics for analysis and calculation. The principle, application scope, advantages and limitations of near infrared spectroscopy and chemometrics are summarized in detail, in addition, their combined applications in the identification of the origin, authenticity, processed products, composition prediction and water content detection of TCM are reviewed. The authors discussed and analyzed the joint application of near-infrared spectroscopy and chemometrics in the field of TCM analysis, and summarized the unique advantages of the combined technology in the field of TCM, which had certain guiding significance for medical workers to better use this technology.

Quality research of Puerariae Lobatae Radix from different habitats with UPLC fingerprint and determination of multi-component content / 中国中药杂志

To establish ultra performance liquid chromatography( UPLC) fingerprint of Puerariae Lobatae Radix from different habitats and simultaneously determine the contents of six isoflavonoids. The UPLC fingerprint analysis and content determination were performed on a Waters ACQUITY UPLC BEH C_(18)( 2. 1 mm×50 mm,1. 7 μm) chromatographic column,with acetonitrile-0. 05% formic acid as mobile phase for gradient elution. The detection wavelength was set at 250 nm; the flow rate was 0. 2 mL·min~(-1); the column temperature was 30 ℃ and the injection volume was 2 μL. Similarity evaluation system for chromatographic fingerprint of traditional Chinese medicine( TCM) was adopted; principal component analysis( PCA) and discriminant analysis by partial least square method( PLS-DA) in Simca-P software were used to identify the differential components in samples from three habitats. The similarity was over 0. 90 in 29 batches of samples,indicating good consistency of the samples. The samples were clustered into 3 categories by PCA and PLS-DA,and six differential components such as puerarin apioside,daidzin,and isoflavoues aglycone were found. The determination results of 6 isoflavones,including 3'-hydroxy puerarin,puerarin,3'-methoxy puerarin,puerarin apioside,daidzin,and isoflavoues aglycone,showed that the content of the same component and the fluctuation range between different components were all different among different habitats. The total content of 6 isoflavones from different regions was Anhui 11. 21% >Henan 10. 97% >Shannxi 9. 38%. The establishment of UPLC fingerprint combined with simultaneous determination of 6 active components provides a more comprehensive reference for quality control and quality evaluation of Puerariae Lobatae Radix.

[Effects of Temperature on FTIR Spectral Characteristics of Renal Tissue in Rats after Death].

OBJECTIVES: To analyse the Fourier transform infrared （FTIR） spectral data of renal tissue at different temperatures in rats after death, and to explore the effects of temperature on the FTIR spectral characteristics of renal tissue. METHODS: The rats were sacrificed by cervical dislocation and placed at 4 ℃, 20 ℃ and 30 ℃. The FTIR spectral data of renal tissue were collected at different time points and analysed by data mining method. RESULTS: The principal component analysis （PCA） results showed that there were significant trends of clustering in the samples of partial time point at 4 ℃, 20 ℃ and 30 ℃. Partial least square （PLS） regression models were established with the spectral data at three temperature groups. The performance of PLS regression models in 20 ℃ and 30 ℃ groups were more superior than that in 4 ℃ group, and the stability of the model in 20 ℃ group was better than that in 30 ℃ group. CONCLUSIONS: There are differences in the FTIR spectral characteristics of renal tissue of rats after death at different temperatures. Temperature has a major impact on the performance of FTIR spectral PLS regression model. Therefore, in order to improve the accuracy of postmortem interval estimation, the effects of temperature on the model should be considered in the related study by spectral method.

Effects of Temperature on FTIR Spectral Characteristics of Renal Tissue in Rats after Death / 法医学杂志

OBJECTIVES@#To analyse the Fourier transform infrared （FTIR） spectral data of renal tissue at different temperatures in rats after death, and to explore the effects of temperature on the FTIR spectral characteristics of renal tissue.@*METHODS@#The rats were sacrificed by cervical dislocation and placed at 4 ℃, 20 ℃ and 30 ℃. The FTIR spectral data of renal tissue were collected at different time points and analysed by data mining method.@*RESULTS@#The principal component analysis （PCA） results showed that there were significant trends of clustering in the samples of partial time point at 4 ℃, 20 ℃ and 30 ℃. Partial least square （PLS） regression models were established with the spectral data at three temperature groups. The performance of PLS regression models in 20 ℃ and 30 ℃ groups were more superior than that in 4 ℃ group, and the stability of the model in 20 ℃ group was better than that in 30 ℃ group.@*CONCLUSIONS@#There are differences in the FTIR spectral characteristics of renal tissue of rats after death at different temperatures. Temperature has a major impact on the performance of FTIR spectral PLS regression model. Therefore, in order to improve the accuracy of postmortem interval estimation, the effects of temperature on the model should be considered in the related study by spectral method.

Rapid Judgement of Blending Endpoint of Jingqi Shuangshen Capsules and Content Determination of Astragaloside Ⅳ by AOTF-NIR / 中国药房

OBJECTIVE:To establish the method for rapid judgement of blending endpoint of Jingqi shuangshen capsules and content determination of astragaloside Ⅳ. METHODS:AOTF-NIR combined with principal component analysis and Moving Block Standard Deviation method was used to identify the blending endpoint. First derivative combined with savitzky-golay filter method were used to spectrum pretreatment. The partial least square method was used to establish quantitative analysis model of the content of astragaloside Ⅳin mixed endpoint sample. The content of astragaloside Ⅳ in mixed endpoint sample was determined by HPLC-ELSD to validate the model. RESULTS:Methodology validation of content determination of astragaloside Ⅳ in mixed material sample and mixed endpoint sample was in line with the requirements. NIR monitoring results showed that the product reached the blending endpoint after 30 min. The results of NIR monitoring were generally consistent with the results of HPLC-ELSD. The principal component dimension of the quantitative model was 9;determination coefficients was 0.954 9;Root Mean Square of Calibration of the model was 0.039 2;Root Mean Square Error of Prediction of the model was 0.042 6. Predicted average value of astragaloside Ⅳ by NIR was 11.74 mg/g,and measured average value of astragaloside Ⅳ by HPLC-ELSD was 11.38 mg/g;average deviation was 3.16%. CONCLUSIONS:AOTF-NIR can rapidly judge the blending endpoint sample of Jingqi shuangshen capsules,rapidly determine the content of astragalosideⅣin mixed endpoint material,improve the quality control level of blending process and shorten blending cycle.

Rapid Determination of Cryptotanshinone in Salvia miltiorrhiza by AOTF-NIDRS / 中国药房

OBJECTIVE:To establish rapid method for content determination of cryptotanshinone in Salvia miltiorrhiza. METHODS:The content of cryptotanshinone in sample was determined by HPLC(as reference value). AOTF-NIDRS combined with PLS was used to establish quantitative correction model for the content of cryptotanshinone in S. miltiorrhiza. According to the results of content determination of cryptotanshinone in samples,35 samples of medicinal material were collected. First-order derivative combined with smoothing filter coefficient method was used to pretreat spectrum,and optimal band range for content determination of cryptotanshinone in sample ranged 1 250-2 150 nm. RESULTS:Methodology validation of content determination of cryptotanshinone in sample was in line with the requirements. Correction mean square deviation of quantitative correction model of cryptotanshinone was 0.014 6,and predicted mean square deviation was 0.022 3,coefficient of association was 0.976 6. The internal verification deviation was 2.41% and the external verification deviation was 4.06%. CONCLUSIONS:This method is rapid,accurate,simple and pollution-free.It can be used for rapid content determination of cryptotanshinone in S.miltiorrhiza.

Rapid Determination of Stilbene Glycoside in Shouwu Pills by Near Infrared Diffuse Reflectance Spectro-photometry / 中国药房

OBJECTIVE:To establish the method for the rapid determination of stilbene glycoside in Shouwu pills. METH-ODS:HPLC method was used to determine the content of stilbene glycoside in Shouwu pills(as measured value). The determina-tion was performed on ODS-C18 column with mobile phase consisted of acetonitrile-water(25:75,V/V)at the flow rate of 0.8 mL/min. The detection wavelength was set at 320 nm,and the column temperature was 30 ℃. The sample size was 10 μL. The partial least square method-near infrared diffuse reflectance spectrophotometry was used to establish quantitative calibration model for pre-dicting the content of stilbene glycoside in Shouwu pills. According to measured value,76 calibration set samples and 24 validation set samples were collected. Standard normalization method and first-order derivative method combined with Savitzky-Goly filter method were used for spectrum pretreatment. The optimal band ranged 9000-4150 cm-1,and main component factor was 12. RE-SULTS:The content determination method of stilbene glycoside in Shouwu pills was in line with the requirements. The correlation coefficients,the root-mean-square error of calibration,the root-mean-square error of predication and the root-mean-square error of cross-validation(RMSECV)of the quantitative calibration model were 0.99190,0.0201,0.0236 and 0.07629. There was no sta-tistical significance between predicted value and measured value(P>0.05). CONCLUSIONS:The method is accurate,stable and simple,and can be used for rapid determination of stilbene glycoside in Shouwu pills.

Determination of Three Compenents in Antodine Injection With Partial Least Square Method / 中国药房

OBJECTIVE:To determine aminophenazone,phenazone and barbital in antodine injection.METHODS:Taking 0.1mol/L NaOH as solvent,the detection data was caculated with partial least square method.RESULTS:The average recoveries were 99.7% for aminophenazone(RSD=0.67%),99.1% for phenazone(RSD=0.76%) and 99.5% for barbital(RSD=0.72%).CONCLUSION:The method is simple,rapid and good in repeatability.