scholarly journals Quantitative Determination of 7 Saikosaponins in Xiaochaihu Granules Using High-Performance Liquid Chromatography with Charged Aerosol Detection

2021 ◽  
Vol 2021 ◽  
pp. 1-7
Author(s):  
Aoxue Liu ◽  
Tongtong Xu ◽  
Wenning Yang ◽  
Dandan Zhou ◽  
Yiwei Sha
Keyword(s):  
High Performance ◽  
Gradient Elution ◽  
Charged Aerosol Detection ◽  
Charged Aerosol ◽  
Relative Standard ◽  
Acid Aqueous Solution ◽  
Bupleuri Radix ◽  
Interday Precision

Bupleuri Radix (Chaihu, in Chinese) is the principal drug in Xiaochaihu granules (XGs) that is a famous Chinese medicine preparation in China. Since previous analytical methods have not focused on the multiactive saikosaponins of Chaihu, it is difficult to effectively control the quality of XG on the market. In this manuscript, the simultaneous determination of 7 saikosaponins (saikosaponins C, I, H, A, B2, G, and B1) in XG by HPLC with charged aerosol detection (CAD) and confirmation by LC-Q-Orbitrap HRMS were described. The saikosaponins were purified on an SPE cartridge and determined on a Waters CORTECTS C18 column (4.6 mm × 150 mm, 2.7 μm) by gradient elution using 0.01% acetic acid aqueous solution and acetonitrile. The results showed good linearity with the r2 values higher than 0.998 for all analytes. The average recoveries at three different concentration levels ranged from 80% to 109% and the intraday and interday precision (relative standard deviations, RSD%) were in the range of 1.0%∼1.9% and 1.4%∼2.1%, respectively. The established HPLC-CAD method was subsequently applied to 15 batches of XG to investigate the batch-to-batch consistency and controllability. The proposed method could potentially be used for the quality control of XG and also be helpful in the quality evaluation of Chaihu and its related preparations.

High Performance Liquid Chromatography Determination of Fentin Acetate Residue in Beet and Soil

2012 ◽  
Vol 550-553 ◽  
pp. 1173-1176
Author(s):  
Hui Qing Sun ◽  
Yi Qiang Li ◽  
Guang Jun Xu ◽  
Xiao Zhen ◽  
Jin Li Xu ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Detectable Level ◽  
Relative Standard ◽  
External Standard ◽  
Detectable Concentration ◽  
Acid Aqueous Solution ◽  
Standard Calibration

Abstract. [Aims] A high performance liquid chromatography (HPLC) was presented for determination of fentin acetate residue in beet and soils. [Methods] Fentin acetate was extracted from beet plants and soils with hydrochloric acid and acetonitrile, followed by a second extraction in dichloromethane, purified by acid aluminium oxide with methanol eluting, then dissolved by concentration and dilution with acetoneitrile. A HPLC with UV detection at 220 nm and a Waters Sun FireTM-C18 column, which was eluted with methanol and 0.5% phosphoric acid aqueous solution and was used based on an external standard calibration curve. [Results] The results showed that the average recoveries were 88.4-95.6% for beet plants and 91.2-91.8% for soils. The relative standard deviations were 2.0-4.5% and 4.3-5.3% respectively. The minimum detectable level was 1.6×10-10g, the lowest detectable concentration was 0.02mg/kg. [Conclusions] The method is convenient and can meet the requirement of residual analysis and also provide reference for other crops.

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 > 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 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.

scholarly journals Simultaneous Determination of Four Active Ingredients inSargentodoxa cuneataby HPLC Coupled with Evaporative Light Scattering Detection

2016 ◽  
Vol 2016 ◽  
pp. 1-7 ◽  
Author(s):  
Di-Hua Li ◽  
Yuan-Shan Lv ◽  
Jun-Hong Liu ◽  
Lei Yang ◽  
Yan Wang ◽  
...  
Keyword(s):  
Light Scattering ◽  
Simultaneous Determination ◽  
Flow Rate ◽  
Evaporative Light Scattering Detection ◽  
Light Scattering Detection ◽  
Evaporative Light Scattering ◽  
Relative Standard ◽  
Acid Aqueous Solution ◽  
Interday Precision

A HPLC coupled with evaporative light scattering detection method had been developed for the simultaneous determination of 3,4-dihydroxyphenylethyl alcohol glycoside, salidroside, chlorogenic acid, and liriodendrin in the stem ofSargentodoxa cuneata. With a C18 column, the analysis was performed using acetonitrile and 0.2% formic acid aqueous solution as mobile phase in gradient program at a flow rate of 0.9 mL/min. The optimum drift tube temperature of evaporative light scattering detection was at 105°C with the air flow rate of 2.5 L/min. The calibration curves showed good linearity during the test ranges. This method was validated for limits of detection and quantification, precision, and reproducibility. The recoveries were within the range of 96.39%–104.64%. The relative standard deviations of intraday and interday precision were less than 2.90% and 3.30%, respectively. The developed method can be successfully used to quantify the four analytes in the stem ofSargentodoxa cuneatafrom various regions in China.

scholarly journals Combined Determination of Succinic Acid and Cetylpyridinium Chloride in Medicinal Films by Gradient High Performance Liquid Chromatography

Medicina ◽  
2021 ◽  
Vol 9 (2) ◽  
pp. 75-88
Author(s):  
O. N. Dvorskaya ◽  
◽  
N. N. Nozhkina ◽  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Succinic Acid ◽  
High Performance ◽  
Cetylpyridinium Chloride ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Gradient Elution Mode

A technique has been developed based on reversed-phase high-performance liquid chromatography with diode-matrix detection for the joint determination of succinic acid and cetylpyridinium chloride in complex action medicinal films. Efficient chromatographic separation of active drug components was achieved in a gradient elution mode on a Luna C18 (2) 100A column (4.6 × 250 mm, 5 µm) using a mobile phase consisting of a 0.1% solution of phosphoric acid and acetonitrile. The detection wavelength was 210 nm for both compounds. The developed method is validated in terms of specificity, linearity, precision, accuracy and can be used to determine the authenticity and quantitative content of succinic acid and cetylpyridinium chloride in the joint presence in assessing the quality of medicinal films.

scholarly journals Simultaneous Determination of Six Major Constituents of the Herbal Formula Insampaedok-san Using HPLC-PDA

2012 ◽  
Vol 2012 ◽  
pp. 1-6 ◽  
Author(s):  
Chang-Seob Seo ◽  
Jung Hoon Kim ◽  
Hyeun-Kyoo Shin
Keyword(s):  
Acetic Acid ◽  
High Performance ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Aqueous Acetic Acid ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Photodiode Array ◽  
Liquid Chromatographic

A simple, rapid, and accurate high-performance liquid chromatographic method was applied to the quantitative analysis of six components of a traditional herbal formulation, Insampaedok-san (ISPDS): liquiritin (1), ferulic acid (2), naringin (3), hesperidin (4), neohesperidin (5), and glycyrrhizin (6). The six components were separated within 35 min using a Gemini C18 column maintained at 40°C. The mobile phase was composed of 1.0% (v/v) aqueous acetic acid (A) and 1.0% (v/v) acetic acid in acetonitrile (B) by gradient elution. The flow rate was 1.0 mL/min and the detector was a photodiode array (PDA) set at 254, 280, and 320 nm. The calibration curves showed good linearity (R2=1.0000) for different concentration ranges. The recovery of each component was in the range of 92.62%–105.96%, with a relative standard deviation (RSD) of less than 4.0%. The RSDs for intra- and interday precision were 0.04%–1.70% and 0.06%–2.56%, respectively. The concentration of each of the six components of ISPDS was in the range 0.72–9.88 mg g−1.

scholarly journals Development of a HPLC-MS/MS Method to Determine the 13 Elements of Semen Cuscutae and Application to a Pharmacokinetic Study in Rats

2019 ◽  
Vol 2019 ◽  
pp. 1-11
Author(s):  
Jiayuan Shen ◽  
Qi Jia ◽  
Xuhua Huang ◽  
Guangzhe Yao ◽  
Wenjuan Ma ◽  
...  
Keyword(s):  
Pharmacokinetic Study ◽  
High Performance ◽  
Rat Plasma ◽  
Pharmacokinetic Parameters ◽  
Plasma Samples ◽  
Mobile Phases ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Interday Precision

This study developed a method for simultaneous determination of 13 elements of Semen Cuscutae (quercitrin, quercetin, hyperoside, caffeic acid, chlorogenic acid, luteolin, apigenin, kaempferol, isoquercitrin, cryptochlorogenic acid, isorhamnetin-3-O-glucoside, astragalin, and rutin) in rat plasma using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) in the negative MRM mode. The analytes were analyzed with CORTECS®C18 column (4.6 × 150 mm, 2.7 μm) with mobile phases consisting of 0.1% formic acid in water (A) and acetonitrile (B). The intra- and interday precision of the target compounds were expressed as relative standard deviation (RSD) in the range of 0.5%–10.4%, and the accuracy of the target compounds was expressed as relative error (RE) not exceeding ±14.5% for all analytes. In the meantime, the extraction recovery of the target compounds in plasma samples ranged from 87.4% to 106.2% and matrix effect from 81.0% to 115.5%. The established method was successfully accomplished for the pharmacokinetic study of the analytes in rat plasma samples following oral administration of Semen Cuscutae extract, and the pharmacokinetic parameters of seven compounds were obtained.

scholarly journals DETERMINATION OF 5H-BENZO[2,3][1,4]OXAZEPINO[5,6-B]INDOLES IN RAT PLASMA BY REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC-ULTRAVIOLET METHOD: APPLICATION TO PHARMACOKINETIC STUDIES

2017 ◽  
Vol 10 (12) ◽  
pp. 425 ◽  
Author(s):  
Ashok K Singh ◽  
Vinit Raj ◽  
Amit Rai ◽  
Amit K Keshari ◽  
Pranesh Kumar ◽  
...  
Keyword(s):  
High Performance ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Rat Plasma ◽  
Reversed Phase ◽  
Pharmacokinetic Studies ◽  
Relative Standard ◽  
Liquid Chromatographic

Objective: Recently, we reported newly synthesized 5H-benzo[2,3][1,4]oxazepino[5,6-b]indole) derivatives and proved their cytotoxicity against hepatocellular carcinoma specific Hep-G2 cell lines. We attempted herein to describe a reversed-phase high-performance liquid chromatographic method for the determination of three most active compounds 6a, 10a, and 15a in rat plasma to predict their pharmacokinetics parameters before in vivo study.Methods: A rapid and sensitive reversed-phase high-performance liquid chromatographic was employed for the determination of 6a, 10a, and 15a in rat plasma. Each compound was separated by a gradient elution of acetonitrile and water with 1 mL/min flow rate. The detector was set at 270, 285, and 275 nm for 6a, 10a, and 15a and the recorded elution times were 2.00, 2.87, and 1.88 min, respectively.Results: The calibration curve was linear with R2 of 0.938, 0.875, and 0.923 over the concentration range of 0.1–50 μg/mL. The inter- and intra-day variations of the assay were lower than 12.26%; the average recovery of 6a, 10a, and 15a was 97.31, 92.56, and 95.23 % with relative standard deviation of 2.12%, 3.25%, and 2.28%, respectively. The Cmax and Tmax were ~ 46.34, 18.56, and 25.65 μg/mL and 2.0, 4.0, and 4.0 h for 6a, 10a, and 15a, respectively, which indicate a robust method of detection in the present experiment.Conclusion: The study suggests that all of the three compounds have a lower rate of absorption, higher volume of distribution, and lower clearance rate, indicating good therapeutic response for in vivo activity. 

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