scholarly journals A High-Sensitivity Analysis Method Of Furanocoumarins In Radix Angelicae Dahuricae By Reverse-Phase High-Performance Liquid Chromatography Coupled With Integrated Pulsed Amperometric Detection

2021 ◽  
Author(s):  
Min-Ji Lee ◽  
Seon-Pyo Hong
Keyword(s):  
High Performance ◽  
Control Measure ◽  
Amperometric Detection ◽  
High Sensitivity ◽  
Gradient Elution ◽  
Quality Control Measure ◽  
Relative Standard ◽  
Sensitivity Analysis Method ◽  
The Mean ◽  
Sensitivity Method

Abstract Radix Angelicae Dahuricae is a traditional Chinese medicine. We developed a high-sensitivity method for detection of furanocoumarins in Radix Angelicae Dahuricae and Gumiganghwal-tang (GMGHT). The six furanocoumarins of Radix Angelicae Dahuricae were sonication-extracted from 50% ethanol for 60 min. Six furanocoumarins were separated through a gradient elution system. The limits of detection of the components were 0.002–0.3 ng (0.2–30 ng/mL). The coefficients of determination were 0.9995–1.0000, all inter-day and intra-day precision values were < 4.9%, and the mean recoveries and relative standard deviations were 96.4%–104.5% and 0.5%–4.8% for Radix Angelicae Dahuricae extract, respectively. Our method does not require any pretreatment steps and exhibits good reproducibility, selectivity, and sensitivity. Therefore, our method will contribute to a Radix Angelicae Dahuricae quality control measure.

scholarly journals Analytical quality by design methodology for botanical raw material analysis: a case study of flavonoids in Genkwa Flos

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Min Kyoung Kim ◽  
Sang Cheol Park ◽  
Geonha Park ◽  
Eunjung Choi ◽  
Yura Ji ◽  
...  
Keyword(s):  
High Performance ◽  
Quality By Design ◽  
Analytical Data ◽  
Gradient Elution ◽  
Raw Material ◽  
Analytical Quality ◽  
Factor Screening ◽  
Column Temperature ◽  
Relative Standard ◽  
Critical Method

AbstractThe present study introduces a systematic approach using analytical quality by design (AQbD) methodology for the development of a qualified liquid chromatographic analytical method, which is a challenge in herbal medicinal products due to the intrinsic complex components of botanical sources. The ultra-high-performance liquid chromatography-photodiode array-mass spectrometry (UHPLC-PDA-MS) technique for 11 flavonoids in Genkwa Flos was utilized through the entire analytical processes, from the risk assessment study to the factor screening test, and finally in method optimization employing central composite design (CCD). In this approach, column temperature and mobile solvent slope were found to be critical method parameters (CMPs) and each of the eleven flavonoid peaks’ resolution values were used as critical method attributes (CMAs) through data mining conversion formulas. An optimum chromatographic method in the design space was calculated by mathematical and response surface methodology (RSM). The established chromatographic condition is as follows: acetonitrile and 0.1% formic acid gradient elution (0–13 min, 10–45%; 13–13.5 min, 45–100%; 13.5–14 min, 100–10%; 14–15 min, 10% acetonitrile), column temperature 28℃, detection wavelength 335 nm, and flow rate 0.35 mL/min using C18 (50 × 2.1 mm, 1.7 μm) column. A validation study was also performed successfully for apigenin 7-O-glucuronide, apigenin, and genkwanin. A few important validation results were as follows: linearity over 0.999 coefficient of correlation, detection limit of 2.87–22.41, quantitation limit of 8.70–67.92, relative standard deviation of precision less than 0.22%, and accuracy between 100.13 and 102.49% for apigenin, genkwanin, and apigenin 7-O-glucuronide. In conclusion, the present design-based approach provide a systematic platform that can be effectively applied to ensure pharmaceutically qualified analytical data from complex natural products based botanical drug.

scholarly journals Simultaneous Rapid Detection of Aflatoxin B1 and Ochratoxin A in Spices Using Lateral Flow Immuno-Chromatographic Assay

Foods ◽  
2021 ◽  
Vol 10 (11) ◽  
pp. 2738
Author(s):  
Xue Zhao ◽  
Xindi Jin ◽  
Zhang Lin ◽  
Qi Guo ◽  
Bin Liu ◽  
...  
Keyword(s):  
Ochratoxin A ◽  
Aflatoxin B1 ◽  
High Performance ◽  
Simultaneous Detection ◽  
High Sensitivity ◽  
Strong Stability ◽  
Test Strip ◽  
Chromatography Analysis ◽  
Relative Standard ◽  
Strip Test

Spices are susceptible to contamination by aflatoxin B1 (AFB1) and ochratoxin A (OTA), which are both mycotoxins with high toxicity and carcinogenicity. In this study, we aimed to develop an immuno-chromatographic strip test for the simultaneous quantification of AFB1 and OTA in spices by spraying the coupled antigens AFB1–ovalbumin (AFB1–OVA) and OTA–ovalbumin (OTA–OVA) on a nitrocellulose membrane. The test strip had high sensitivity, good specificity, and strong stability. The detection limits of these two mycotoxins in Chinese prickly ash, pepper, chili, cinnamon, and aniseed were 5 μg/kg. The false positivity rate was 2%, and the false negativity rate was 0%. The maximum coefficient of variation was 4.28% between batches and 5.72% within batches. The average recovery rates of AFB1 and OTA in spices were 81.2–113.7% and 82.2–118.6%, respectively, and the relative standard deviation (RSD) was <10%. The actual sample detection was consistent with high performance liquid chromatography analysis results. Therefore, the immuno-chromatographic test strips developed in this study can be used for the on-site simultaneous detection of AFB1 and OTA in spices. This method would allow the relevant regulatory agencies to strengthen supervision in an effort to reduce the possible human health hazards of such contaminated spices.

Validation of HPLC Method for Determination of Histamine in Human Immunoglobulin Formulations

2020 ◽  
Vol 103 (5) ◽  
pp. 1223-1229
Author(s):  
Michikazu Tanio ◽  
Toru Nakamura ◽  
Hideki Kusunoki ◽  
Kyohei Ideguchi ◽  
Kazuyuki Nakashima ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
High Performance ◽  
Gradient Elution ◽  
Hplc Method ◽  
Human Immunoglobulin ◽  
Histamine Dihydrochloride ◽  
Relative Standard

Abstract Background Histamine fixed-immunoglobulin formulations, which consisted of 0.15 µg of histamine dihydrochloride and 12 mg of human immunoglobulin in a vial, are used for anti-allergic treatments, and controlling the amounts of histamine in the formulations is essential to avoid histamine intoxication. Objective A high-performance liquid chromatography (HPLC) method for determination of histamine contents of the formulations was established and validated. Methods Histamine extracted from the formulation was labeled with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate and was analyzed by gradient elution HPLC with UV detection at 260 nm. Results The method showed linearity in the range 0.8–2.4 µM (R &gt; 0.999), accuracy (100.1–105.8% recovery), and precision (relative standard deviation ≤ 1.93%). The validated method was applied for five lots of the pharmaceutical, and their histamine contents were determined to be 0.149–0.155 µg/vial. Conclusions These results indicated that the validated method is useful to control amounts of histamine in biopharmaceutical products. Highlights The HPLC method was developed for quantitative determination of histamine content of the histamine fixed-immunoglobulin formulations.

scholarly journals Determination of cyanide in bamboo shoots by microdiffusion combined with ion chromatography–pulsed amperometric detection

2018 ◽  
Vol 5 (4) ◽  
pp. 172128 ◽  
Author(s):  
Ming Ding ◽  
Kailiang Wang
Keyword(s):  
Ion Chromatography ◽  
Limit Of Detection ◽  
Correlation Coefficients ◽  
Amperometric Detection ◽  
High Sensitivity ◽  
Practical Method ◽  
Pulsed Amperometric Detection ◽  
Bamboo Shoots ◽  
Relative Standard

A practical method for the determination of cyanide in bamboo shoots has been developed using microdiffusion preparation integrated with ion chromatography–pulsed amperometric detection (IC-PAD). Cyanide was released from bamboo shoots after Conway cell microdiffusion, and then analysed by IC-PAD. In comparison with the previously reported methods, derivatization and ion-pairing agent addition were not required in this proposed microdiffusion combined with IC-PAD method. The microdiffusion parameters were optimized including hydrolysis systems, temperature, time, and so on. Under the optimum conditions, the linear range of the calibration curve for cyanide was 0.2–200.0 µg kg −1 with satisfactory correlation coefficients of 0.9996 and the limit of detection was 0.2 µg kg −1 ( S/N  = 3). The spiked recovery range was from 92.8 to 98.6%. The intra-day and inter-day relative standard deviations of cyanide were 2.7–14.9% and 3.0–18.3%, respectively. This method was proved to be convenient in operation with high sensitivity, precision and accuracy, and was successfully applied in the determination of cyanide in bamboo shoot samples.

scholarly journals High-Performance Thin-Layer Chromatography with Densitometry for the Determination of Ciprofloxacin and Impurities in Drugs

2005 ◽  
Vol 88 (5) ◽  
pp. 1530-1536 ◽  
Author(s):  
Jan Krzek ◽  
Urszula Hubicka ◽  
Justyna Szczepańczyk
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
High Sensitivity ◽  
Good Precision ◽  
Relative Standard ◽  
Tlc Plates ◽  
Quantitative Analyses

Abstract A thin-layer chromatographic (TLC)-densitometric method has been developed for identification and quantification of ciprofloxacin (Rf = 0.61) and an ethylenediamine compound (Rf = 0.42), a desfluoro compound (Rf = 0.48), by-compound A (Rf = 0.53), and fluoroquinolonic acid (Rf = 0.68) as ciprofloxacin degradation products in pharmaceutical preparations. By using chloroform–methanol–25% ammonia (43 + 43 + 14, v/v/v) as the mobile phase and silica gel 60 F254 high-performance TLC plates as the stationary phase, it was possible to separate individual constituents that, when subjected to ultraviolet (UV) densitometric analysis at 330 nm for fluoroquinolonic acid and 277 nm for the other compounds, gave well developed peaks allowing easy qualitative and quantitative analyses. DMSO–methanol (1 + 1) was used to extract drug constituents. The method showed high sensitivity (limit of detection 10 to 44 ng), a wide linearity range (3 to 20 μg/mL), and good precision (2.32 to 6.46% relative standard deviation) and accuracy (percentage recoveries 98.62 to 101.52%) for individual constituents.

scholarly journals Simultaneous Determination of Eight Synthetic Permitted and Five Commonly Encountered Nonpermitted Food Colors in Various Food Matrixes by High-Performance Liquid Chromatography

2010 ◽  
Vol 93 (5) ◽  
pp. 1503-1514 ◽  
Author(s):  
Sumita Dixit ◽  
Subhash K Khanna ◽  
Mukul Das
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
High Sensitivity ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Food Category ◽  
Food Commodities ◽  
Food Colors

Abstract A simple and sensitive HPLC method has been developed for the simultaneous determination of eight permitted food colors and five commonly encountered nonpermitted colors in various food commodities, including sugar-, fat-, and starch-based food matrixes. The method uses a specific food category-based cleanup/treatment procedure before color extraction to avoid the interference of food matrixes, and to obtain the optimal color extraction. Analysis was performed on a reversed-phase C18 -Bondapak column with ammonium acetate and acetonitrile gradient elution as the mobile phase; a programmable max-specific visible detection was used to monitor colors to obtain the higher sensitivity and expanded scope needed for multicolor blends having diverse absorption maxima. All colors showed good linearity, with regression coefficients of 0.99740.9999. The LOD and LOQ values ranged from 0.01 to 0.12 mg/L, and from 0.04 to 0.83 mg/L or mg/kg, respectively. The intraday and interday precision tests produced good RSD values, and the recoveries from different food matrixes ranged from 82 to 104%. The method offers high sensitivity for analysis of a wide variety of food matrixes containing a broad scope of multicolor blends. Two nonpermitted colors, orange II and metanil yellow, were found. Also, a number of samples contained permitted colors at levels two-to seven-fold higher than those prescribed.

Serotonin and its N-Acetylated and Acidic Derivatives in Insect Brain as Determined by High-Performance Liquid Chromatography with Electrochemical Detection

1993 ◽  
Vol 28 (1) ◽  
pp. 16-24 ◽  
Author(s):  
R. Vieira ◽  
M. Aldegunde
Keyword(s):  
Analytical Method ◽  
High Performance ◽  
Amperometric Detection ◽  
High Sensitivity ◽  
Hplc Method ◽  
Insect Brain ◽  
Oxidative Deamination ◽  
Wide Range ◽  
Hydrodynamic Voltammetry

The determination of serotonin (5-HT), N-acetylserotonin (NAS) and 5-hydroxy-3-indoleacetic acid (5-HIAA) in single brains of two acridids (Paracinema tricolor and Oedipoda caerulescens) was accomplished using a HPLC method combined with amperometric detection. A hydrodynamic voltammetry approach was used to assess the identity of each peak by comparing the voltammograms of standards and those of samples. The analytical method gave satisfactory reproducibility and sensitivity, and detected levels of 5-HT, NAS and 5-HIAA as low as 29, 55 and 10 fmol, respectively. This high sensitivity together with the simplicity of sample processing make the present analytical method suitable for a wide range of studies concerning indoleamine analyses in the insect nervous system. In both acridids, 5-HT showed the largest quantities, while its derivatives occurred in extremely low amounts. The results suggest that N-acetylation of 5-HT is quantitatively preferred to oxidative deamination in both species (NAS levels were 4-fold those of 5-HIAA). The relative importance of each catabolic pathway is discussed as related to physiological and genetic aspects.

Determination of β -Sitosterol with Chemical Course and Material Applications in Jatropha Seed Oil by High Performance Liquid Chromatography

2012 ◽  
Vol 577 ◽  
pp. 69-72 ◽  
Author(s):  
Shu Yu Liu ◽  
Anaerguli Maihemuti
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Seed Oil ◽  
Reversed Phase ◽  
Analytical Recovery ◽  
Relative Standard ◽  
The Mean ◽  
Jatropha Seed

A simple and rapid high performance liquid chromatography (HPLC) assay was developed to identify and measure theβ-sitosterol with chemical course and material applications in jatropha seed oil. The stigmasterol was isolated with a good selectivity by HPLC employing reversed phase C18 columns. The components were separated by mobile phase of methanol-water (99/1, v/v) and detected at 205nm. The quantitation of the stigmasterol was reproducible and the method relative standard deviation is 1.1%. The mean analytical recovery was 96.2%.

scholarly journals A novel method of reversed migration capillary electrophoresis for determination of linear alkylbenzene sulfonates

2021 ◽  
Vol 12 (1) ◽  
Author(s):  
Zhuo Huang ◽  
Weike Wang ◽  
Lingxian Xie ◽  
Li Lin
Keyword(s):  
Capillary Electrophoresis ◽  
High Performance ◽  
Ph Value ◽  
High Sensitivity ◽  
Chromatography Method ◽  
Linear Alkylbenzene ◽  
Relative Standard ◽  
Linear Alkylbenzene Sulfonates ◽  
Liquid Chromatography Method ◽  
And Migration

AbstractA reversed migration capillary electrophoresis (RMCE) has been developed to determine linear alkylbenzene sulfonates (LAS). The sample stacking and separation conditions have been systematically investigated and optimized under reversed separation voltage at a low pH value. The separation effect of LAS homologs has been greatly improved based on the relative motion of electrophoresis and electroosmotic flow. RMCE demonstrates a good linear range of 0.1 mg/l to 10.0 mg/l, and the detection limit of LAS homologs reaches 0.001–0.004 mg/l. The relative standard deviations (n=6) of peak area and migration time were 2.25–4.40% and 0.67–0.75%, respectively. RMCE has also been applied for LAS detection in practical wastewater. The results show RMCE exhibits easy pretreatment, fast detection, high sensitivity, good peak shapes and resolution, and less solvent consumption, compared with the established high-performance liquid chromatography method.

scholarly journals Determination of 5-nitro-2-furaldehyde as marker residue for nitrofurazone treatment in farmed shrimps and with addressing the use of a novel internal standard

2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Qiang Wang ◽  
Xu-Feng Wang ◽  
Yong-Yuan Jiang ◽  
Zhi-Guang Li ◽  
Nan Cai ◽  
...  
Keyword(s):  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Negative Ionization ◽  
Ultrasonic Manipulation

AbstractWe developed a significantly improved ultra-high performance liquid chromatography-tandem mass spectrometry method for determination of 5-nitro-2-furaldehyde (NF) as a surrogate using a novel internal standard for the detection of nitrofurazone. We used 2,4-dinitrophenylhydrazine derivatization and furfural as the internal standard. Derivatization was easily performed in HCl using ultrasonic manipulation for 5 min followed by liquid extraction using ethyl acetate. The samples were concentrated and purified using reverse phase and alumina cartridges in tandem. The derivatives were separated using a linear gradient elution on a C18 column with methanol and water as the mobile phase in negative ionization mode and multiple reaction monitoring. Under the optimized conditions, the calibration curves were linear from 0.2 to 20 μg/L with correlation coefficients >0.999. Mean recoveries were 80.8 to 104.4% with the intra- and inter-day relative standard deviations <15% at spiking levels of 0.1 to 10 μg/kg. The limits of detection and quantification were 0.05 and 0.1 μg/kg, respectively. This method is a robust tool for the identification and quantitative determination of NF in shrimp samples.

Sign in / Sign up

Export Citation Format

Share Document