Analysis of 8-methoxypsoralen by high-performance liquid chromatography

1990 ◽  
Vol 36 (11) ◽  
pp. 1956-1957 ◽  
Author(s):  
C H Ketchum ◽  
C A Robinson ◽  
S T Huang

Abstract We report a simple and rapid procedure for assaying 8-methoxypsoralen (8-MOP) in plasma by high-performance liquid chromatography (HPLC). The standard curve for the assay is linear for 8-MOP from 15 to 500 micrograms/L (y = 0.002x-0.01, r = 0.99) with a lower limit of detection of 1.5 micrograms/L. Intra-assay precision (CV) was 6.0% at the 100 micrograms/L concentration and 10.0% at 50 micrograms/L (n = 30 each). Interassay precision was 6.4% at 100 micrograms/L and 7.0% at 50 micrograms/L (n = 50 each). Extraction recovery of 8-MOP was 98%. Common antiarrhythmics, sedatives, and hypnotics were found not to interfere.

2013 ◽  
Vol 83 (2) ◽  
pp. 122-128 ◽  
Author(s):  
Cécile Renaud ◽  
Jacques Berger ◽  
Arnaud Laillou ◽  
Sylvie Avallone

Vitamin A deficiency is still one of the major public health problems in least developed countries. Fortification of vegetable oils is a strategy implemented worldwide to prevent this deficiency. For a fortification program to be effective, regular monitoring is necessary to control food quality in the producing units. The reference methods for vitamin A quantification are expensive and time-consuming. A rapid method should be useful for regular assessment of vitamin A in the oil industry. A portable device was compared to high-performance liquid chromatography (HPLC) for three plant oils (rapeseed, groundnut, and soya). The device presented a good linearity from 3 to 30 mg retinol equivalents per kg (mg RE.kg- 1). Its limits of detection and quantification were 3 mg RE.kg- 1 for groundnut and rapeseed oils and 4 mg RE.kg- 1 for soya oil. The intra-assay precision ranged from 1.48 % to 3.98 %, considered satisfactory. Accuracy estimated by the root mean squares error ranged from 3.99 to 5.49 and revealed a lower precision than HPLC (0.4 to 2.25). Although it offers less precision than HPLC, the device estimates quickly the vitamin A content of the tested oils from 3 or 4 to 15 mg RE.kg- 1.


Author(s):  
Raju Chandra ◽  
Manisha Pant ◽  
Harchan Singh ◽  
Deepak Kumar ◽  
Ashwani Sanghi

A reliable and reproducible reversed-phase high performance liquid chromatography (RP-HPLC) was developed for the quantitative determination of Remipril drug content from marketed bulk tablets. The active ingredient of Remipril separation achieved with C18 column using the methanol water mobile phase in the ratio of 40:60 (v/v). The active ingredient of the drug content quantify with UV detector at 215 nm. The retention time of Remipril is 5.63 min. A good linearity relation (R2=0.999) was obtained between drug concentration and average peak areas. The limit of detection and limit of quantification of the instrument were calculated 0.03 and 0.09 µg/mL, respectively. The accuracy of the method validation was determined 102.72% by recoveries method.


2021 ◽  
pp. 1-11
Author(s):  
Sultan M. Alshahrani ◽  
John Mark Christensen

This study was designed to develop and validate a simple and efficient high performance liquid chromatography (HPLC) method to determine flunixin concentrations in Asian elephant’s (Elephas maximus) plasma. Flunixin was administered orally at a dose of 0.8 mg/kg, and blood samples were collected. Flunixin extraction was performed by adding an equal amount of acetonitrile to plasma and centrifuging at 4500 rpm for 25 minutes. The supernatant was removed, and flunixin was analyzed using HPLC-UV detection. Two methods were developed and tested utilizing two different mobile phases either with or without adding methanol (ACN: H2O vs. ACN: H2O: MeOH). Both methods showed excellent linearity and reproducibility. The limit of detection was 0.05 ug/ml and limit of quantification was 0.1 ug/ml. the efficiency of flunixin recovery was maximized by the addition of methanol to mobile phase (ACN: H2O: MeOH as 50:30:20) at 95% in comparison to 23% without methanol. In conclusion, adding methanol to HPLC methods for extraction of flunixin from elephants’ plasma yielded higher recovery rate than without methanol.


Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.


1975 ◽  
Vol 145 (3) ◽  
pp. 517-526 ◽  
Author(s):  
F B Jungalwala ◽  
R J Turel ◽  
J E Evans ◽  
R H McCluer

A highly sensitive method for the separation and quantitative measurement of phospholipids containing primary amino groups, such as phosphatidylethanolamine, phosphatidylserine and lysophosphatidylethanolamine, is described. The method involves a simple and quantitative derivative formation of the phospholipids containing amino groups to their u.v.-absorbing biphenylcarbonyl derivatives. These have molar extinction coefficients of about 23,000 at 268nm. The phospholipid derivatives are then separated and non-destructively determined by high-performance liquid chromatography. The amino phospholipids containing vinyl ether bonds (plasmalogens) can be determined separately from the diacyl- and alkylacyl-amino phospholipids. The lower limit of detection by high-performance liquid-chromatographic analysis of the phospholipid derivatives is about 10-13pmol or 0.3-0.4ng of phospholipid P. The quantitative range of derivative formation and analysis by high-performance liquid chromatography of the phospholipids containing amino groups was shown to be 10-500nmol. The method was shown to be applicable to the analysis of phospholipids containing amino groups in tissue samples.


2020 ◽  
Vol 58 (5) ◽  
pp. 471-476 ◽  
Author(s):  
Jiong Li ◽  
Jinyan Gong ◽  
Haina Yuan ◽  
Gongnian Xiao ◽  
Hongqing Wang ◽  
...  

Abstract This study established a rapid and reliable method to determine chloramphenicol (CAP), thiamphenicol (TAP) and florfenicol (FF) residues in Chinese gelatin medicines. CAP, TAP and FF were extracted from medicine samples using 2% (v/v) ammonium hydroxide in acetonitrile. Trypsin was used to eliminate the matrix effect caused by protein components in gelatin medicines, whereas anhydrous sodium sulfate, C18-N and NH2-PSA adsorbents were applied to reduce matrix effect induced by other components. The analytical method of these drugs was optimized on ultra high-performance liquid chromatography-mass spectrometer (UHPLC-MS/MS) through the analysis of their standard linearity and regression. The optimized extraction and analytical method were validated in one Chinese gelatin medicine sample (Colla corii asini, E Jiao) with three fortification levels (2, 5 and 10 μg/kg), and the recoveries of these drug residues ranged of 87.6–102.7%. The limit of detection and quantification of CAP, TAP and FF in the sample were 0.2 and 0.5 μg/kg, 0.4 and 1.5 μg/kg, and 0.5 and 1.5 μg/kg, respectively. A total of 30 Chinese gelatin medicine samples were analyzed using the established method. No drug residues were found in these samples except for one Testudinis Carapacis et Plastri (1.67 μg/kg FF) and one turtle shell glue (2.55 μg/kg FF).


Author(s):  
Kanan G Gamit ◽  
Niraj Y Vyas ◽  
Nishit D Patel ◽  
Manan A Raval

Objective: A study was aimed to estimate guggulsterone-Z (GZ) in Gokshuradi Guggulu (GG).Methods: An analytical method was developed and validated using Waters Alliance high-performance liquid chromatography system (Empower software), equipped with photodiode array detector. Separation was achieved using Phenomenex, C-18 (250 mm×4.6 mm, 5 μ) column. Mobile phase consisted of acetonitrile:water (70:30,v/v). Flow rate was set to 1 ml/min and detection was performed at 251 nm.Results and Discussion: Validation parameters such as linearity, precision, accuracy, limit of detection, limit of quantification, and robustness were performed. Amount of GZ was estimated using linearity equation.Conclusion: GG was found to contain 0.815±0.03 g% w/w GZ. Validated method may be used as one of the parameters to standardize the formulation.


2011 ◽  
Vol 140 ◽  
pp. 296-301 ◽  
Author(s):  
Cai Mei Wu ◽  
Hong Min Yuan ◽  
Gang Jia ◽  
Zhi Sheng Wang ◽  
Xiu Qun Wu

A reversed high performance liquid chromatography method was developed for the quantitative determination of mimosine and 2,3-DHP in leaves ofLeucaena Leucocephala. Mimosine and 2,3DHP were extracted using 0.1N HCl.The chromatograph conditions were investigated and optimized. The optimal HPLC conditions as follows: Agilent HC-C18 column (4.6×150mm,5μm) was used at 30°C. The method used a variable wavelength UV detector at 280nm, the mobile phase consisted of 0.2 % (w/v) orthophosphoric acid and methanol, the gradient elution was adopted. The injection volume was 10μL. The linearity is favorable in the range of 1.0 to 50μg mL-1with a correlation coefficient of 0.99998 for mimosine and 0.99902 for 2,3DHP. Under the optimal conditions, the method limit of detection (LOD) of mimosine and 2,3DHP were 0.40mg/kg and 0.55mg/kg respectively. The recovery of mimosine was 87.00-94.70% with the RSD (n=5) of 2.75-3.81% in the spiked levels 0,1, 5, 20mg/g. At the same time, the recovery of 2,3DHP was 88-95.4% with the RSD (n=5) of 2.24-4.90%. The method was found to be simple, sensitive, fast and accurate, and has been applied successfully for the quantitative detection of mimosine and 2,3-DHP in leaves ofLeucaena Leucocephala, plasma and excretion of ruminant.


Author(s):  
BAITHA PALANGGATAN MAGGADANI ◽  
JIHAN YASMINA ◽  
HARMITA HARMITA

Objective: Whitening cream is a cosmetic that contains ingredients that can alleviate hyperpigmentation. Tranexamic acid (TA) is one of the potentialanti-pigmentation agents that work through inhibiting plasmin. TA is used in cosmetic formulations at a concentration of 2.5% as a whitening andmoisturizing agent. To date, research on TA in both cosmetics and other pharmaceutical products using high-performance liquid chromatography(HPLC) has not been done directly (without derivatization). Therefore, this study aimed to develop a simple and rapid analytical method for TA(without derivatization) in cosmetic cream samples using reverse-phase HPLC and water as a solvent.Methods: Optimization was conducted by evaluating several parameters that affect sample extraction, as well as composition and mobile phasetypes. The optimal method must fulfill suitability and validation requirements. The optimal method should be able to detect and quantify TA in creamsamples without derivatization.Results: The optimal analysis condition used a ultraviolet detector at a wavelength of 210 nm, acetonitrile: double-distilled water: phosphoric acid(64:34:2) as the mobile phase and a flow rate of 0.8 mL/min. The retention time of the analyte occurred in the 2nd min.Conclusion: The analytical method that met the validation requirements was characterized using parameters such as accuracy, precision, linearity,selectivity, limit, of detection, and limit of quantitation. This method is applicable for analyzing TA content in samples with a concentration of 1.02%.


2008 ◽  
Vol 3 (5) ◽  
pp. 1934578X0800300 ◽  
Author(s):  
Hui-Jun Li ◽  
Zheng-Ming Qian ◽  
Ping Li ◽  
Mei-Ting Ren ◽  
Jun Chen ◽  
...  

A new high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS) method has been developed for the simultaneous determination of nine major compounds, namely chlorogenic acid (1), caffeic acid (2), sweroside (3), loganin (4), secoxyloganin (5), 3,5-di- O-caffeoyl quinic acid (6), luteolin-7- O-glucoside (7), rutin (8) and 3,4-di- O-caffeoyl quinic acid (9), in Caulis Lonicerae Japonicae (CLJ), a commonly used traditional Chinese medicinal herb. The separation was achieved on a C-18 column (250 × 4.6 mm, 5.0 μm) with a column temperature of 30°C and a flow-rate of 0.8 mL/min. The mobile phase was composed of (A) aqueous formic acid (0.1%, v/v) and (B) methanol, using a gradient elution of 30% B for 0-13 min, 30–40% B for 13–17 min, and 40–49% B for 17–30 min. The limit of detection ( S/ N = 3) ranged from 0.8 to 5.1 ng/mL and the limit of quantification ( S/ N = 10) varied from 3.4 to 16.9 ng/mL. All calibration curves showed good linear regression ( r2 > 0.9976) within the test ranges. The intra- and inter-day precisions, as determined from sample solutions, were below 2.2 and 4.3%, respectively. The recoveries for nine compounds were within 91.3 and 104.2%. This proposed method has been successfully applied to evaluation of commercial samples of CLJ from different markets in China, which provides a new basis of assessment of the quality of the herbal drug.


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