Detection of 9α-OH-AD Prepared by Biotransformation

2013 ◽  
Vol 821-822 ◽  
pp. 1005-1008
Author(s):  
Li Min Ma ◽  
Li Cui ◽  
Yu Hang Zhao
Keyword(s):  
Quality Control ◽  
Correlation Coefficient ◽  
Flow Rate ◽  
Standard Method ◽  
Mobile Phase ◽  
Average Recovery ◽  
Rp Hplc ◽  
External Standard Method ◽  
External Standard

Detection of 9а-OH-AD prepared by biotransformation by RP-HPLC directly was studied.The detection is performed on a Kromasil 100-5C18(4.6×250mm) column, using methanol:water(7:3,v/v)as mobile phase,0.8mL•min-1flow rate and external standard method,deteced at 242nm.There is a good line correlaction between peak and content in range of 0.01-0.20g/L,the correlation coefficient is 0.9942,the average recovery is 99.09% with a relative stand deviation of 0.89%(n=5).The method is simple,stable,accurate and reliable for quality control of 9а-OH-AD.

scholarly journals Establishment of the Quantitative Analysis of Multiindex in Euphorbia lathyris by the Single Marker Method for Euphorbia lathyris Based on the Quality by Design Concept

2021 ◽  
Vol 2021 ◽  
pp. 1-8
Author(s):  
Feng Xuehua ◽  
Zhou Guangjiao ◽  
Tao Ali
Keyword(s):  
Flow Rate ◽  
Standard Method ◽  
Mobile Phase ◽  
Column Temperature ◽  
Injection Volume ◽  
External Standard Method ◽  
Relative Standard ◽  
Significant Difference ◽  
External Standard ◽  
Euphorbia Lathyris

Methods. The influences of methanol proportion, flow rate, column temperature, and injection volume in the mobile phase on the chromatographic resolution of chromatographic peak of euphorbia factor L1 were experimentally studied via Plackett–Burman design, and the key analysis parameters were screened out; the key analysis parameters were optimized through the central composite design, and the chromatographic analysis conditions were established. Euphorbia factor L1 was taken as the internal reference to construct the relative correction factors for L3 and L4 relative to L1, and their contents were calculated, thus realizing the QAMS. Meanwhile, the euphorbia factor L3 and euphorbia factor L4 were determined using the external standard method, and the differences of values measured by the external standard method from the values predicted by the QAMS method were compared, in an effort to verify the accuracy and feasibility of the QAMS method. Results. The methanol proportion and column temperature in the mobile phase were the key analysis parameters P < 0.05 , and the chromatographic conditions were determined as follows. The methanol/water ratio, column temperature, detection wavelength, flow rate, and injection volume were 60 : 40, 30°C, 275 nm, 1.0 mL/min, and 10 μL, respectively. A total of 20 batches of samples were determined by the QAMS method and external standard method; the relative standard deviations (RSDs) of L3 and L4 determination results were less than 2.0%, without any significant difference. Conclusion. The QbD-based QAMS method can be used to determine the contents of euphorbia factor L3 and euphorbia factor L4 in Euphorbia lathyris L., and it is accurate and feasible.

Detection of L-Tert-Leucine in the Enzyme-Catalyzed Reaction System

2013 ◽  
Vol 641-642 ◽  
pp. 717-720
Author(s):  
Sheng Deng ◽  
Li Cui ◽  
Li Min Ma
Keyword(s):  
Quality Control ◽  
Correlation Coefficient ◽  
Flow Rate ◽  
Catalytic Reaction ◽  
Reaction System ◽  
Direct Determination ◽  
Average Recovery ◽  
Enzyme Catalytic Reaction

Direct Determination of L-Ter-Leucine in Enzyme Catalytic Reaction System by HPLC Was Studied. the Detection Were Performed on a Kromasil 700-5C18 Column Using a Eluant Containing 0.25% (NH4)H2PO4 and 100% Methanol (V((NH4)H2PO4):V(methanol)=100:5) with the Flow Rate of 0.8 Ml/min at,detection Wavelength of 205nm. there Was a Good Line Correlation between Peak Area and Contents in the Rang of 0.2-10 Mg/ml, the Correlation Coefficient Was 0.9986, the Average Recovery Was 98.88% with a Relative Stand Deviation of 0.78% (n=5). this Method Is Simple, Stable, Accurate and Reliable for the Quality Control of L–ter-Leucine.

Degradation Profiling of Lisinopril and Hydrochlorothiazide by RP- HPLC method with QbD Approach

2021 ◽  
pp. 270-274
Author(s):  
Kalleshvar P. Jatte ◽  
R. D. Chakole ◽  
M. S. Charde
Keyword(s):  
Particle Size ◽  
Quality Control ◽  
Flow Rate ◽  
Mobile Phase ◽  
Dosage Form ◽  
Quality By Design ◽  
Hplc Method ◽  
Rp Hplc ◽  
Tablet Dosage ◽  
Gradient Mode

RP-HPLC method was developed for the estimation of Lisinopril and Hydrochlorothiazide in tablet dosage form with the help of Quality by Design (QbD) approaches. In this method concentration of each drug was obtained by using the absorptivity values calculated for drug wavelength 226.0 nm and solving the equation. The RP-HPLC method was performed C18-(100mm x 4.6 mm,)2.5 μm particle size in gradient mode, and the sample was analysed using methanol 45.0 ml and 55.0 ml (pH 3.3 0.05% OPA with TEA) as a mobile phase at a flow rate of 0.8 ml/min and detection at nm. By the retention time for Lisinopril and Hydrochlorothiazide found 3.39 and 4.59 min respectively. Validation related the method is specific, rapid, accurate, precise, reliable, and reproducible. Calibration plots by both HPLC were linear over the 5-25 and 12.5-62.5 μg/ml for Lisinopril and Hydrochlorothiazide respectively, and recoveries from tablet dosage form were between 99.02 and 100.00 %. The method can be used for routine of the quality control in pharmaceuticals. The degradation profiling of Lisinopril and Hydrochlorothiazide were also carried out.

Determination of Paeoniflorin and Paeonol in Houyinan Tablet by UPLC

2012 ◽  
Vol 581-582 ◽  
pp. 68-72
Author(s):  
Chu Qin Yu ◽  
Hua Qing Lin ◽  
Yue Han Hou ◽  
Zhong Feng Shi ◽  
Di Shi Lin
Keyword(s):  
Quality Control ◽  
Simultaneous Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
Gradient Elution ◽  
The Other ◽  
Column Temperature ◽  
Average Recovery ◽  
Injection Volume

In this study, our purpose was to establish a UPLC method for the simultaneous determination of Paeoniflorin and Paeonol in Houyinan Tablet. The separation was performed on Acquity BEH C18 column(2.1mm×100mm,1.7μm), the mobile phase was acetonitrile-water with gradient elution at a flow rate of 0.2 mL•min-1, the detection wavelength was 230nm, the column temperature was 30°Cand the injection volume was 2μL. Paeoniflorin and Paeonol reached effective separation with the other components in this chromatographic conditions. Paeoniflorin and Paeonol were linear within the range of 0.0406~0.4064μg(r=0.9999) and 0.0426~0.4256μg (r=0.9999), respectively. The average recovery was 99.82% and 100.6%. The results of method validation indicated that the method was simple,quick,accurate, specific and less solvent consumption. It can be used for the quality control of Houyinan Tablet.

Determination of Patulin Residues in Canned Fruits by HPLC

2014 ◽  
Vol 1004-1005 ◽  
pp. 936-940
Author(s):  
Ling Lin ◽  
Chun Liang Yang ◽  
Shao Dong Zeng ◽  
Qi Li ◽  
Hong Bin Guo
Keyword(s):  
Standard Method ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Constant Volume ◽  
Uv Detection ◽  
External Standard Method ◽  
Fruit Samples ◽  
External Standard ◽  
Sensitive Method

A sensitive method for determining residues of patulin in canned fruits was established by HPLC.Canned fruit samples were extracted with acetonitrile and purified through multifunctional cleanup column.Collected purifying liquids and blowed N2 to nearly dry,and then using the mobile phase to dissolve and constant volume, and were determined by UV detection at 276 nm with external standard method for quantitative, the recovery rates of patulin in canned fruits were 80%~95%, The RSD were of 2.2%~6.5%,the limit of detection was 0.012 μg /kg for patulin.

Liquid Chromatographic Assay of Bentazon Formulations

1993 ◽  
Vol 76 (2) ◽  
pp. 387-389
Author(s):  
Thomas M Schmitt
Keyword(s):  
Standard Method ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
Active Agent ◽  
Reversed Phase ◽  
External Standard Method ◽  
Liquid Chromatographic Method ◽  
External Standard ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A reversed-phase liquid chromatographic method is presented for determining the active agent in technical bentazon and in aqueous formulations of the sodium salt of bentazon. The procedure is an isocratic, external standard method specifying an octadecylsilyl column, an acetate-buffered mobile phase of methanol-water, and UV detection. The 340 nm detection wavelength eliminates interference from formulation impurities.

Matrine Determination in Compound Sophora Alopecuroides Suppositories by High-Performance Liquid Chromatography

2013 ◽  
Vol 634-638 ◽  
pp. 1001-1004
Author(s):  
Hui Xiang Hu ◽  
Xuan Zhang ◽  
Zhimin Zhang
Keyword(s):  
Quality Control ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Average Recovery ◽  
Sophora Alopecuroides ◽  
Rp Hplc

The determination of matrine in compound sophora alopecuroides suppositories was carried out by reversed-phase high-performance liquid chromatography(RP-HPLC). Elite ODS C18(250mm×4.5mm, 5µm) column was used and acetonitrile -anhydrous ethanol-water-triethy lamine (15:22.5:62.5:0.01) was selected as the mobile phase. Meanwhile the detection wavelength 215nm was used. The linearity of matrine was in the range of 0.74-5.18µg，r=0.9991，and the average recovery was 98.52%，RSD was 1.54%. The method was proved to be simple, accurate, sensitive and reliable. It can be used for the quality control of compound sophora alopecuroides suppositories.

scholarly journals Box-Behnken Assisted Validation and Optimization of an RP-HPLC Method for Simultaneous Determination of Domperidone and Lansoprazole

Separations ◽  
2021 ◽  
Vol 8 (1) ◽  
pp. 5
Author(s):  
Mohd Afzal ◽  
Mohd. Muddassir ◽  
Abdullah Alarifi ◽  
Mohammed Tahir Ansari
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Box Behnken Design ◽  
Rp Hplc ◽  
System Suitability ◽  
Method Optimization ◽  
Key Variables

A highly specific, accurate, and simple RP-HPLC technique was developed for the real-time quantification of domperidone (DOMP) and lansoprazole (LANS) in commercial formulations. Chromatographic studies were performed using a Luna C8(2), 5 μm, 100Å, column (250 × 4.6 mm, Phenomenex) with a mobile phase composed of acetonitrile/2 mM ammonium acetate (51:49 v/v), pH 6.7. The flow rate was 1 mL·min−1 with UV detection at 289 nm. Linearity was observed within the range of 4–36 µg·mL−1 for domperidone and 2–18 µg·mL−1 for lansoprazole. Method optimization was achieved using Box-Behnken design software, in which three key variables were examined, namely, the flow rate (A), the composition of the mobile phase (B), and the pH (C). The retention time (Y1 and Y3) and the peak area (Y2 and Y4) were taken as the response parameters. We observed that slight alterations in the mobile phase and the flow rate influenced the outcome, whereas the pH exerted no effect. Method validation featured various ICH parameters including linearity, limit of detection (LOD), accuracy, precision, ruggedness, robustness, stability, and system suitability. This method is potentially useful for the analysis of commercial formulations and laboratory preparations.

scholarly journals RP-HPLC Determination of Raloxifene in Pharmaceuticl Tablets

2006 ◽  
Vol 3 (1) ◽  
pp. 60-64 ◽  
Author(s):  
P. Venkata Reddy ◽  
B. Sudha Rani ◽  
G. Srinu Babu ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

A reverse phase HPLC method is developed for the determination of Raloxifene in pharmaceutical dosage forms. Chromatography was carried out on an inertsil C18 column using a mixture of acetonitrile and phosphate buffer (30:70 v/v) as the mobile phase at a flow rate of 1 mL/min. Detection was carried out at 290 nm .The retention time of the drug was 10.609 min. The method produced linear responses in the concentration range of 0.5-200 µg/mL of Raloxifene. The method was found to be applicable for determination of the drug in tablets.

SIMULTANEOUS ESTIMATION OF CURCUMIN AND GEFITINIB IN BULK AND TISSUE SAMPLES (PLASMA AND BRAIN HOMOGENATE) BY RP-HPLC: APPLICATION TO A DISTRIBUTION STUDY

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (07) ◽  
pp. 59-68
Author(s):  
H Mahajan ◽  
S Savale ◽  
P Nerkar ◽  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Internal Standard ◽  
Brain Homogenate ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Bulk Analysis ◽  
Experimental Conditions ◽  
Rp Hplc

The present study was aimed at developing a Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC) method for simultaneous determination of curcumin (CRM) and gefitinib (GFT) in bulk, plasma and brain homogenate. hydrochlorothiazide was used as an internal standard (IS). A new simple, rapid, selective, precise and accurate RP-HPLC method has been developed. The separation was achieved by using C-18 column (Qualisil BDS C18, 250 mm x 4.6 mm I.D.) coupled with a guard column of silica, mobile phase consisted of acetonitrile: water with 0.1% formic acid (30:70 v/v). The flow rate was 0.2 ml/min and the drug was detected using PDA detector at the wavelength of 242 nm. The experimental conditions, including the diluting solvent, mobile phase composition, column saturation and flow rate, were optimised to provide high-resolution and reproducible peaks. The method was developed and tested for linearity range of 10-60 μg/mL for bulk analysis and 200-800 ng/mL for plasma and brain homogenate. The developed method was validated as per ICH guidelines, in terms of linearity, application of the proposed method to bulk sample, recovery, precision, repeatability, ruggedness, sensitivity (LOD and LOQ) and robustness and stability study (short and long-term stabilities, freeze/thaw stability, post-preparative). The low value of % RSD showed that the method was precise within the acceptance limit of 2%. The developed method was successfully applied for the analysis of the drug in bulk as well as various marketed formulation and drug in plasma and brain distribution studies.

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