ABSTRACT
This study established a method for rapid quantification of terpene lactone, bilobalide, ginkgolide C, ginkgolide A and ginkgolide B in the chromatographic process of Ginkgo Folium based on near infrared spectroscopy(NIRS). The effects of competitive adaptive reweighting sampling(CARS), random frog(RF), and synergy interval partial least squares(siPLS) on the performance of partial least squares regression(PLSR) model were compared to the reference values measured by HPLC. Among them, the correlation coefficients of prediction(Rp) of validation sets of terpene lactone, bilobalide, and ginkgolide C were all higher than 0.98, and the relative standard errors of prediction(RSEPs) were 5.87%, 6.90% and 6.63%, respectively. Aiming at ginkgolide A and ginkgolide B with relatively low content, the genetic algorithm joint extreme learning machine(GA-ELM) was used to establish the optimized quantitative analysis model. Compared with CARS-PLSR model, the CARS-GA-ELM models of ginkgolide A and ginkgolide B exhibited a reduction in RSEP from 15.65% to 8.52% and from 21.28% to 10.84%, respectively, which met the needs of quantitative ana-lysis. It has been proved that NIRS can be used for the rapid detection of various lactone components in the chromatographic process of Ginkgo Folium.
Subject(s)
Chromatography, High Pressure Liquid , Ginkgo biloba , Lactones/analysis , Least-Squares Analysis , Spectroscopy, Near-Infrared/methodsABSTRACT
Objective To establish a rapid determination model based on near-infrared spectroscopy (NIRS) for glycyrrhizic acid and liquiritin in Glycyrrhizae Radix et Rhizoma Yinpian. Methods The contents of glycyrrhizic acid and liquiritin in Glycyrrhizae Radix et Rhizoma Yinpian from different places of origin were determined by high performance liquid chromatography (HPLC) as reference values. At the same time 2 200-2 049, 1 750-1 450, 1 151-1 001 nm and 1 795-1 475, 1 395-1 293, 1 125-1 030 nm wavelength ranges of near-infrared spectra were selected to establish the rapid determination model by combining partial least squares (PLS) regression analysis with cross validation method. Results The correlation coefficient and root-mean-squares error of cross validation of the established content calibration model were 0.980 and 0.184 for glycyrrhizic acid, and 0.919 and 0.144 for liquiritin, respectively. Conclusion The NIRS-PLS method is convenient, rapid and nondestructive for the content determination of glycyrrhizic acid and liquiritin for large number of Glycyrrhizae Radix et Rhizoma Yinpian, which provides a new and feasible method for the rapid quality evaluation of Glycyrrhizae Radix et Rhizoma Yinpian.
ABSTRACT
Objective@#To develop a rapid detection method for 21 elements in urine with inductively coupled plasma mass spectrometry (ICP-MS) .@*Methods@#The urine samples were directly diluted 20 times by 1% HNO3, and detected by ICP-MS, Indium, Yttrium, and Lutecium were used as on-line internal standard. Fe was analyzed by Dynamic Reaction Cell (DRC) mode, As, Cr, V and Zn were analyzed by collision cell technology (CCT) mode, and Be, Mn, Ni, Cd, Sn, Bi, Pb, Re, Sb, W, Li, Cu, Se, Sr, Mo were analyzed by standard mode. Dynamic band-pass tuning (DBT) was used to eliminate interference for Fe.@*Results@#All the elements have good linearity in their determination range, with the correlation coefficient r>0.999 5. The limits of detection of the 21 elements were in the range of 0.017-11.14 μg/L. The inter-precision (relative standard deviation, RSD) was less than 9.96%, and the intra-precision was less than 13.90% (except As RSD<18.91%) . The spike recovery of all elements fell within 81.1%-116.4%.@*Conclusion@#The method was proved to be simple, fast, and accurate, and met the needs of testing requirements of large amounts of specimens.
ABSTRACT
Objective: To established a rapid nondestructive determination method for the multi-marker constituents in Angelica sinensis by near infrared spectroscopy (NIRS) combined with the partial least squares (PLS) method in order to improve the quality control for A. sinensis. Methods: A total of 108 batches of A. sinensis from different origins were collected for the research. An Ultra performance liquid chromatography (UPLC) method was established to measure the content of the seven components in A. sinensis, which were adopted as the reference value. And the integrating sphere diffuse reflection mode was employed to collect the NIR spectrum. The quantitative calibration model between the near infrared spectrum and the reference content of each component to be measured was established by PLS and other chemometrics methods. Each part of the modeling process was optimized respectively, including the selection of calibration set and validation set, different pretreatment methods and different spectral section. Results: The correlation coefficient for calibration set of chlorogenic acid, ferulic acid, isochlorogenic acid A, ligustilide, butylidenephthalide, senkyunolide I and levistilide A were 0.937 6, 0.970 2, 0.963 4, 0.991 1, 0.962 4, 0.966 6 and 0.947 6, respectively; The root mean square error of prediction (RMSEP) were 0.072 1, 0.038 9, 0.011 3, 0.483 0, 0.017 5, 0.178 0 and 0.097 0, respectively. The predicted values of NIRS models and the measured values of UPLC showed a good linear relation, which presented a great prediction ability of the models. Conclusion: The methods of NIRS combined with PLS can be applied for the rapid content determination of seven components in A. sinensis including chlorogenic acid, ferulic acid, isochlorogenic acid A, ligustilide, butylidenephthalide, senkyunolide I and levistilide A, which is proved to be simple and reliable.
ABSTRACT
OBJECTIVE： To establish a method for rapid determination of total phenylethanoid glycosides and total iridoid glycosides in the root of Rehmannia glutinosa. METHODS： The contents of total phenylethanoid glycosides and total iridoid glycosides in medicinal material samples were determined by UV spectrophotometry. Quantitative model of total phenylethanoid glycosides and total iridoid glycosides in medicinal samples was established by NIRS-PLS method. The optimal pretreatment spectra were multivariate scattering correction combined with first derivative method， standard normalization combined with first derivative method. The optimum spectral ranged from 6 703.35-11 065.54 cm－1 and 3 999.63-9 102.36 cm－1. The optimum principal factor number were 10 and 7. RESULTS： The content determination of total phenylethanoid glycosides and total iridoid glycosides in medicinal material samples was proved to meet the requirements by methodological experience. The internal cross validation determination coefficients of total phenylethanoid glycosides and total iridoid glycosides were 0.998 2 and 0.980 9. The correction of root mean square error was 0.032 7 and 0.186 0. The root mean square error of prediction were 0.035 5 and 0.035 1. The root mean square error of cross validation were 0.256 9 and 0.574 3. The predicted values of total phenylethanol glycosides and total iridoid glycosides were 0.268％-1.636％ and 3.424％-6.978％， respectively； the determination value of them were 0.299％-1.629％ and 3.431％-6.952％， respectively； the absolute deviations were －0.042％-0.067％ and －0.111％-0.088％， respectively；the relative deviations were －0.819％-0.076％、－2.257％-1.672％， respectively；There was no statistical significance between predicted values and measured values （P＞0.05）. CONCLUSIONS： The method is accurate and simple. The method can be used for the rapid determination of total phenylethanoid glycosides and total iridoid glycosides in different germplasms of R. glutinosa.
ABSTRACT
Objective To establish a rapid and nondestructive method for the determination of multi-components in Salvia miltiorrhiza to improve the quality control of S. miltiorrhiza based on Near infrared spectroscopy combined with partial least squares (PLS) method. Methods A total of 106 batches of S. miltiorrhiza samples from different origins were collected. The content of 11 components (tanshinol sodium, protocatechuic aldehyde, caffeic acid, rosmarinic acid, alkannic acid, salvianolic acid B, salvianolic acid A, dihydrotanshinone, tanshinone I, cryptotanshinone, and tanshinone IIA) in all of the samples which was conducted as the reference value were determined by a UPLC method established in the previous research. And the NIRS spectrum were obtained under the integrating sphere diffuse reflection mode. The different processes of modeling were optimized by partial least squares (PLS) and other chemometrics methods, including the selection of calibration set and validation set, different pretreatment method, different spectral section, and the determination of factors. A linear quantitative calibration model between the near infrared spectrum and the content of the components to be measured was tried to be established so that the content of the components could be measured by NIRS rapidly. Results The predicted value of NIRS and the measured value of UPLC of five components in S. miltiorrhiza, including salvianolic acid B, dihydrotanshinone, tanshinone I, cryptotanshinone, and tanshinone IIA, presented a good linearity, indicating the calibration models had a preferable forecast results. The correlation coefficient were 0.981 1, 0.936 3, 0.960 5, 0.910 9, 0.978 0 respectively, and the mean and square deviation of the prediction set (RMSEP) were 0.957 0, 0.037 7, 0.041 6, 0.114, 0.063 9, respectively; But the model of the other constituents failed to reach the quantitative level. Conclusion The content of salvianolic acid B, dihydrotanshinone, tanshinone I, cryptotanshinone, tanshinone IIA in S. miltiorrhiza can be determined rapidly and nondestructive by the NIRS combined with PLS method, which lays a foundation for the rapid and field determination method for the medicinal materials and decoction pieces of S. miltiorrhiza.
ABSTRACT
OBJECTIVE:To establish the method for rapid determination of nuezhenoside in Salvia miltiorrhiza.METHODS:The contents of salvianolic acid B,rosmarinic acid,lithospermic acid and tanshinone (tanshinone Ⅱ A+tanshinone Ⅰ +cryptotanshinone) were determined by HPLC (as reference value).Quantitative model for the contents of above components was established by partial least square (PLS)-NIR spectra.According to the reference value,143 samples were collected and the spectrum was pretreated by first-order derivative.The optimal range of wave band for salvianolic acid B,rosmarinic acid,oxalic acid and tanshinone were 6 773.98-3 981.12,6 670.85-3 996.54,8 544.66-3 936.28,8 188.06-3 875.31 cm-1.RESULTS:The methodology for the content determination of salvianolic acid B,rosmarinic acid,oxalic acid and tanshinone were in line with the requirement.The coefficient (R2) of internal cross validation for quantitative correction model of salvianolic acid B,rosmarinic acid,oxalic acid and tanshinone were 0.919 0,0.832 2,0.821 5,0.925 6.The deviation of corrected mean square roots were 4.46,0.48,1.34,0.71,respectively.The R2 values of external validation were 0.852 6,0.957 3,0.819 3,0.953 1,respectively;and mean square root of prediction error (RMSEP)were 9.77,0.28,0.94,0.63,respectively.CONCLUSIONS:The method is rapid,accurate,simple and pollution-free,and can be used for rapid determination of multi-maker ingredients in S.miltiorrhiza.
ABSTRACT
To establish a rapid determination method of six flavonoids:catechin,rutin,myricetin,quercetin,kaempferol and isorhamnetin,from seabuckthorn leaves by RP-HPLC-DAD.The seabuckthorn leaves were first degreased by petroleum ether,extracted by ethanol,and determined by RP-HPLC-DAD.The six flavonoids were separated and eluted by a Shimadzu C18(150 mm ×2.1 mm,5 μm) column with methanol-water (0.1％ phos phoric acid) (60∶ 40) at a flow rate of 1.0 mL/min.The detection wavelength were as follow:catechin 208 nm,rutin 257 nm,myricetin 373 nm,quercetin 371 nm,kaempferol 367 nm,and isorhamnetin 371 nm,respectively.The injection volume was 20 μL.The contents of the six flavonoids were in the range of 0.47 to 30.00 μ,g/mL with good linearity.The validation of the method,including precision,stability and recovery rate,was acceptable.The established method can be used for fast determination of the content of six flavonoids in seabuckthorn leaves.
ABSTRACT
Objective To establish a new method with near-infrared (NIR) spectroscopy to determine the total content of emodin, chrysophanol, rhein, aloeemodin, and physcion. NIR was used in this study to provide rapid and nondestructive analysis results. Methods In the first place, HPLC was used to measure the total content of emodin, chrysophanol, rhein, aloe-emodin and physcion in Rhei Radix et Rhizoma (RR) as a reference. In the second place, the spectral regions, regression methods, pretreatment methods, and partial least squares (PLS) factors were compared to increase the feasibility of the model. In the last, the root mean square error of calibration (RMSEC), root mean square error of cross validation (RMSECV), root mean square error of prediction (RMSEP), and correlation coefficient (r) were used as assessment parameters. Results PLS with first derivative pretreatment in the ranges of 4242-5581 cm−1, 5885-6233 cm−1 and 6394-7011 cm−1 provided the best results. The RMSEC and RMSEP obtained were 0.134 and 0.226 respectively. The according determination coefficients of the quantitative model were 0.99 and 0.94. Conclusion NIR spectroscopy as a quick and nondestructive analytical method may be used to determine the total content of emodin, chrysophanol, rhein, aloeemodin, and physcion for the quality control of RR.
ABSTRACT
Objective:To develop a method for the rapid determination of CaSO4 ·2H2 O in gypsum by Raman spectra. Methods:Totally 40 batches of gypsum from different origins were used as the training set, compared with the results by ENTA titration, and OPUS software was used to establish a quantitative analysis model of CaSO4 ·2H2 O in gypsum by Raman spectra. Results:The estab-lished quantitative analysis model could provide a good prediction result rapidly when the content was between 97. 93% and 99. 81%. Conclusion:The method is accurate, fast and simple, which can be developed as an analysis method for CaSO4 ·2H2 O in gypsum.
ABSTRACT
This paper was aimed to study the method of rapid determination of total flavonoids in Chrysanthemum of different processing methods by near infrared spectroscopy (NIRS). The Chrysanthemum was dried by three different processes. The three methods were directly drying, drying after steamed and drying after fry, respectively. The determination of total flavonoids in Chrysanthemum by different processing methods was produced by using UV-Vis spectrophotometry. Collecting the NIRS spectra of Chrysanthemum, the quantitative analysis model of total flavonoids content in Chrysanthemum of different processing methods was established by partial least square (PLS) and the model was validated. The correlation coefficient (R2), the root-mean-square error of calibration (RMSEC) and the root-mean-square error of prediction (RMSEP) were 0.996 19, 0.104 and 0.168, respectively. The correlation coefficient of predication (r) was 0.979 3 which state that the prediction was accurate. The method of NIRS had the advantage of fast determination, simple operation and high accuracy of prediction, and could be used for rapid determination of total flavonoids content in Chrysanthemum of different processing methods.
ABSTRACT
Objective To establish a method of automatic analysis of iodide in drinking water.Methods In accordance with the principles of the National Standard Methods Standard Testing Methods for Dringking Water (GB 5750-2006),the reagent concentration and the ratio of dosage were optimized; the national standard artificial colorimetric detection of iodide in drinking water was substituted by automatic biochemical analyzer colorimetric analysis procedure; the accuracy and the precision of the new method were observed and compared with the National Standard Methods.Results In determination of iodide in drinking water by using automatic biochemical analyzer,the best linear ranges of the standard curve:low concentrations 0-＜ 50 μg/L with a correlation coefficient of 0.999 1,and the detection limit was 0.4 μg/L; at high concentrations of 50-500 μg/L the correlation coefficient was 0.999 3,and the detection limit was 4.0 μg/L.The coefficient of variation was 2.2％-4.2％ and the recovery was between 98.6％-1035％.Compared with the National Standard Methods,the difference was not statistically significant (t =0.97-1.70,all P ＞ 0.05).Conclusions The method of determination of iodide in drinking water by using automatic biochemical analyzer is successfully established.The accuracy and the precision of the method can meet the quality requirements of water quality analysis.
ABSTRACT
Oleaginous microbial strains were cultivated to identify the best oil-producing strain amongst Yarrowia lipolytica (CGMCC 2.1398), Lipomyces starkeyi (CGMCC 2.1608), Rhodosporidium toruloides (CGMCC 2.1389), Mortierella isabellina (CGMCC 3.3410), Cunninghamella blakeleana (CGMCC 3.970), and Mycobacterium QJ311. A method for rapid determination of oil content and fatty acid composition was established to identify the optimum oil-producing strains. This method had a relative standard deviation of 4.09%, an average recovery ratio of 97.09% and a detection limit of 0.1–1.0 g. Mortierella isabellina CGMCC 3.3410 was identified as the best oil-producing strain amongst the six strains tested, with a total biomass of 75 g/10 L and a lipid content of 35%. A rapid screening method of oleaginous microorganisms is discussed for the first time.
ABSTRACT
AIM: To determine baicalin of scutellaria-extract rapidly by FT-NIRS and data analysis software. METHODS: The correction model was set up based on partial least square and was used to predict baicalin of scutellaria-extract in the samples. RESULTS: Cross validation and test samples determination showed that the co-rrelation coefficient(R2) of this correction model was 95.05,the RMSECV was 0.861,respectively. CONCLUSION: It is fast and convenient.The correction model could be used to predict baicalin of scutellaria-extract rapidly.It can offer reference to content determination of other extracts of Chinese herbs.
ABSTRACT
Objective:To establish a simple,fast,exact and sensitive method to determine the quality of arteannuin on the spot.Methods:In contrast to the results based on HPLC in the aid of soxhlet extraction,an on-the-spot determination of Artemisinin by UV aided by ul-trasonic extraction was proposed.Results:The content of Artemisinin extracted with on-the-spot method for rapid determination is com-puted by equation:MRD(mg.g-1)=(A?V?2.2984)(/As?3)+1.2067.Conclusion:This method with ultrasonic extraction of artean-nuin and UV determination simplified the procedure and saved work time.It proved to be an satisfactory method for determination of arteannuin.