Quantitative Analysis Of Active Ingredient Research Articles

A green ultrasonic-assisted micellar extraction coupled with ultra-high performance liquid chromatography with photodiode array method for quantitative analysis of active ingredients in Yangxinshi Tablet

An efficient and green ultrasonic-assisted micellar extraction method coupled with ultra-high performance liquid chromatography with photodiode array detection (UHPLC-PDA) was developed for the multi-ingredients quantitative analysis of Yangxinshi Tablet (YXST). The active ingredients were extracted from YXST using trehalose lipid biosurfactant solution as an environmentally friendly extraction solution. The response surface methodology (RSM) based on Box-Behnken design (BBD) was utilized to seek for the optimum extraction conditions of target analytes. When the concentration of trehalose lipid solution was 7 mg/mL, the liquid to solid was 125:1 (mL:g) and the extraction time was 40 min, the total extraction yield of eleven compounds (including puerarin, daidzin, ferulic acid, calycosin-7-O-β-D-glucoside, tetrahydropalmatine, coptisine, epiberberine, jatrorrhizine, berberine, palmatine chloride and icariin) obtained the maximum value. The relative standard deviations (RSD) of intra-day and inter-day precision were all less than 5.0%. The recoveries of all analytes were in the range of 95.1%−104% with the RSDs were all below 3.0%. Consequently, the ultrasonic-assisted micellar extraction coupled with UHPLC-PDA method could be successfully and efficiently applied to the extraction and quantitative analysis of target components in YXST.

Qualitative and quantitative analysis of active ingredients in secondary residue of Turkish gall treated with simulated gastrointestinal environment in vitro

Qualitative and quantitative analysis of active ingredients in secondary residue of Turkish gall treated with simulated gastrointestinal environment in vitro

A Rapid and Sensitive Method for the Simultaneous Determination of Multipolar Compounds in Plant Tea by Supercritical Fluid Chromatography Coupled to Ion Mobility Quadrupole Time-of-Flight Mass Spectrometry.

In this study, matrix solid phase dispersion (MSPD) microextraction combined with supercritical fluid chromatography-ion mobility quadrupole time-of-flight mass spectrometry (SFC/IM-QTOF-MS) was used to analyze the multipolar compounds in plant tea. The parameters of stationary phase, mobile phase, make-up solution, temperature, and back pressure were optimized. The target analytes were gradient eluted in 8 min by supercritical CO2 on a Zorbax RX-SIL column. Collisional Cross Section (CCS) values for single and multiple fields were measured. A series of validation studies were carried out under the optimal conditions, and the linear relationship and reproducibility were good. The limits of detection were 1.4 (Scoparone (1))~70 (Naringenin (4)) ng/mL, and the limits of quantification were 4.7 (Scoparone (1))~241 (Naringenin (4)) ng/mL. The recoveries of most compounds ranged from 60.7% to 127%. As a consequence, the proposed method was used for the separation and quantitative analysis of active ingredients in caulis dendrobii.

A Rapid and Sensitive Method for the Simultaneous Determination of Multipolar Compounds in Caulis Dendrobii by Supercritical Fluid Chromatography Coupled to Ion Mobility Quadrupole Time-of-Flight Mass Spectrometry

In this study, matrix solid phase dispersion (MSPD) microextraction combined with supercritical fluid chromatography-ion mobility quadrupole time-of-flight mass spectrometry (SFC/IM-QTOF-MS) was used to analyze the multipolar compounds in caulis dendrobii. The parameters of stationary phase, mobile phase, make-up solution, temperature and back pressure were optimized. The target analytes were gradient eluted in 8 min by supercritical CO2 on Zorbax RX-SIL column. Collisional Cross Section (CCS) values for single and multiple fields were measured. A series of validation studies were carried out under the optimal conditions, and the linear relationship and reproducibility were good. The limits of detection were 1.415~8.824 ng/mL, and the limits of quantification were 4.717~29.412 ng/mL. The recoveries of most compounds ranged from 86.51% to 107.2%. As a consequence, the proposed method was used for the separation and quantitative analysis of active ingredients in caulis dendrobii.

차나무 추출물 함유 유기농업자재 중 주성분 정량분석법 확립

차나무 추출물 함유 유기농업자재 중 주성분 정량분석법 확립

Rapid and quantitative determination of fentanyls and pharmaceuticals from powdered drug samples by paper spray mass spectrometry.

Paper spray mass spectrometry is presented as a direct, quantitative tool for the measurement of pharmaceutical drugs and a variety of fentanyl analogs in solid samples and powder slurries with the ultimate goal of providing meaningful harm-reduction drug checking. Method development and validation was carried out for fentanyl analog slurries as a proxy for street drug samples. Lower limits of quantitation were determined to be 3.6-7.4ng/g for fentanyl analogs in the pharmaceutical slurry matrix. Using 1mg of solid sample, the method can quantify picogram quantities of these drugs, well below required thresholds for even the most potent fentanyl analogs. Quality control samples were prepared and used to assess method validity according to the Scientific Working Group for Forensic Toxicology (SWGTOX) guidelines. Performance metrics for both precision and accuracy were found to be within SWGTOX-recommended guidelines. Additionally, pharmaceutical tablets were used to demonstrate the applicability of the developed paper spray methodology for the direct qualitative and quantitative analysis of active ingredients in pharmaceutical powders deposited directly onto the paper spray substrate. A proposed workflow for rapid solid drug sample measurements is presented with potential applications for point-of-use street drug measurements and other solid sample matrices.

Exploiting third-order advantage using four-way calibration method for direct quantitative analysis of active ingredients of Schisandra chinensis in DMEM by processing four-way excitation–emission-solvent fluorescence data

In this paper, a new strategy of introducing an extra solvent mode in the three-way EEMs data to construct a four-way EX–EM-solvent-samples data set was used in order to investigate the ‘third-order advantage’ by comparing the performances of two four-way calibration algorithms with those of two three-way calibration algorithms. The results of the self-weighted alternating normalized residue fitting (SWANRF) and the parallel factor analysis (PARAFAC) algorithms were both disappointing in this work due to serious collinearity and high background interference. In contrast, the satisfactory results (average recovery, 100.0–107.4% and standard deviation, 1.0–3.0%) were obtained by the third-order calibration methods based on both four-way self-weighted alternating normalized residue fitting (four-way SWANRF) and four-way parallel factor analysis (four-way PARAFAC) algorithms. In addition, for prediction of Dulbecco's modified eagle medium (DMEM) samples, the root-mean-square error of prediction (RMSEP) values for schizandrol B obtained from two three-way calibration algorithms were 60.91 and 35.46μgmL−1 with 80% ethanol in the aqueous solvent, which were obviously much larger than these (0.0832 and 0.0825μgmL−1) obtained using two algorithms of the four-way calibration. The results demonstrated that third-order calibration can extract more inherent information from the data, and can easily solve the problems of serious collinearity and high background interference. In short, among the advantages of this method over the existing methods, low cost, non-toxic and non-destructive analysis can be cited.

The original Croatian pharmacopoeia from 1901.

The second edition of the Croato-Slavonian Pharmacopoeia was published in Zagreb in 1901. As the original scientific work of two university professors, Gustav Janecek and Julije Domac, the Pharmacopoeia had strong scientific foundations and introduced a number of innovations. For the first time, a pharmacopoeia prescribed optical rotation for the examination of essential oils, introduced the quantitative analysis of active ingredients in galenic preparations, standardized the boiling points at the atmospheric pressure of 760 mm Hg, and was the only one to prescribe antidotes for herbal drugs and preparations which may cause poisoning. It received extremely positive reviews from the most prominent European pharmaceutical experts. It was written in two languages, Latin and Croatian, and had a wider significance, since it reflected the aspirations of the Croatian people for independence.

Detection of Chlorogenic Acid in Honeysuckle Using Infrared-Assisted Extraction Followed by Capillary Electrophoresis with UV Detector

In this study, a novel infrared-assisted extraction method coupled capillary electrophoresis (CE) is employed to determine chlorogenic acid from a traditional Chinese medicine (TCM), honeysuckle. The effects of pH and the concentration of the running buffer, separation voltage, injection time, IR irradiation time, and anhydrous ethanol in the extraction concentration were investigated. The optimal conditions were as follows: extraction time, 30 min; extraction solvent, 80% (v/v) ethanol in water solution; and 50 mmol/L borate buffer (pH 8.7) was used as the running buffer at a separation voltage of 16 kV. The samples were injected electrokinetically at 16 kV for 8 s. Good linearity (r(2) > 0.9996) was observed over the concentration ranges investigated, and the stability of the solutions was high. Recoveries of the chlorogenic acid were from 95.53% to 106.62%, and the relative standard deviation was below 4.1%. By using this novel IR-assisted extraction method, a higher extraction efficiency than those extracted with conventional heat-reflux extraction was found. The developed IR-assisted extraction method is simple, low-cost, and efficient, offering a great promise for the quick determination of active compounds in TCM. The results indicated that IR-assisted extraction followed by CE is a reliable method for quantitative analysis of active ingredient in TCM.

Analysis and Evaluation on Chemical Composition of the Larch Bark

In this paper, Chinese larch bark and different areas of Korean larch bark chemical composition and quantitative analysis of active ingredients, and with several plant resources in the total flavonoids were compared and evaluated. The results showed that: Korean larch bark of ash content (1.34%) lower, phenethyl alcohol extract (16.17%), proanthocyanidins (3.84%), total flavonoids(16.59%) and dihydro-quercetin (4.87% ) the highest. The total flavonoid content is more higher than the development of herbal extracts of total flavonoids. Therefore, the bark is a great potential for development of renewable resources.

Reliable and fast quantitative analysis of active ingredient in pharmaceutical suspension using Raman spectroscopy

The concentration of acetaminophen in a turbid pharmaceutical suspension has been measured successfully using Raman spectroscopy. The spectrometer was equipped with a large spot probe which enabled the coverage of a representative area during sampling. This wide area illumination (WAI) scheme (coverage area 28.3 mm 2) for Raman data collection proved to be more reliable for the compositional determination of these pharmaceutical suspensions, especially when the samples were turbid. The reproducibility of measurement using the WAI scheme was compared to that of using a conventional small-spot scheme which employed a much smaller illumination area (about 100 μm spot size). A layer of isobutyric anhydride was placed in front of the sample vials to correct the variation in the Raman intensity due to the fluctuation of laser power. Corrections were accomplished using the isolated carbonyl band of isobutyric anhydride. The acetaminophen concentrations of prediction samples were accurately estimated using a partial least squares (PLS) calibration model. The prediction accuracy was maintained even with changes in laser power. It was noted that the prediction performance was somewhat degraded for turbid suspensions with high acetaminophen contents. When comparing the results of reproducibility obtained with the WAI scheme and those obtained using the conventional scheme, it was concluded that the quantitative determination of the active pharmaceutical ingredient (API) in turbid suspensions is much improved when employing a larger laser coverage area. This is presumably due to the improvement in representative sampling.

Determination of active ingredient within pharmaceutical preparations using flow injection mass spectrometry

Two separate pharmaceutical blends, one containing 2% caffeine by weight, the other containing 2% creatine by weight, and 200 mg caffeine tablets were examined in this study. The purpose of the analyses was to determine the feasibility of using flow injection mass spectrometry for the quantitative analysis of active ingredient within a drug product or other form of pharmaceutical preparation. For more precise and accurate measurements, it was necessary to incorporate an internal reference within the samples. Further, flow injection analysis showed to provide quicker, more facile method development than the application of chromatographic separation. Samples were analyzed over an analyte concentration range of 5.0–15.0 μg/mL. Analyte selectivity was obtained through the observance of the ( M + H) + ions generated by positive electrospray ionization of each of the analytes ( m/ z 195 for caffeine and m/ z 132 for creatine), and accurate quantitation was achieved by determining the ratio of the analyte response versus the response of the incorporated reference compound. Sample-to-sample precision in these measurements was less than 3%, recovery values were shown to be accurate to within ±3% of the actual values, and both analytical methods proved to be linear over the assay range ( R 2 ≥ 0.999). Due to the excellent selectivity and low detection limits available to mass spectrometric detection, flow injection mass spectrometric analysis could be particularly applicable for analysis of formulations that contain either low doses of active ingredient, active ingredient with low solubility, or active ingredient that does not possess a strong chromophore. Additionally, this type of methodology shows to be conducive for rapid method development.