scholarly journals PENGUJIAN VALIDASI ANALISIS KADAR ANDROGRAFOLID SECARA KROMATOGRAFI CAIR KINERJA TINGGI (KCKT) DENGAN ELUASI GRADIEN TERHADAP EKSTRAK HERBA SAMBILOTO (ANDROGRAPHIS PANICULATA NESS)

2005 ◽  
Vol 11 (1) ◽  
pp. 73-76
Author(s):  
Toetik Aryani

Andrographolide of Andrographis paniculata Nees have been isolated and determined Extraction was carried out by maceration with ethanol as solvent. The concentration of Andrographolide was determined by HPLC method. The eluation was carried by out gradiently using methanol: water as an eluent and UV spectrophotometer at maks 228 as detector. The result of HPLC analysis are selectivity more than 1.2–1.5, r was 0.9937, precision was KV less than 10 percent; accuracy more than 90 percent, DL was 0.075, QL was 0.50 and PW less than F table. Andrographolide content of Andrographis paniculata Nees from Banyuwangi was 6.25 percent, Kediri was 14.69 percent and Surabaya was 6.83 percent.

1986 ◽  
Vol 49 (5) ◽  
pp. 383-388 ◽  
Author(s):  
PETER SPORNS ◽  
SUET KWAN ◽  
LAWRENCE A. ROTH

Oxytetracycline (OTC), also known commercially as Terramycin, was determined to be more stable in honey than in buffered aqueous solutions at similar pH values and temperatures. A rapid high performance liquid chromatography (HPLC) method was developed to detect and quantitate OTC using a 1:1 dilution (wt/wt) of honey samples in water. Using 355 nm as the wavelength of detection, amounts as low as 0.5 μg/ml could be detected in the above solution. The limits of detection were lowered considerably by a double extraction procedure.


2018 ◽  
Vol 1 (1) ◽  
pp. 19
Author(s):  
Vevi Maritha ◽  
Lukman Labasy

The aim of the present study was to develop and validate HPLC method for the simultaneous assay of metamizole, thiamine and pyridoxine in tablet. Metamizole is a substance that is easily hydrolyzed in the precence of water and oxygen. To inhibit the hydrolysis of metamizole during sample preparation prior to HPLC analysis, sodium sulfite is added and its optimum concentration was investigated. The chromatographic system includes a RP C8(2) column (150x4.6 mm, 5 µm particle size) in conjunction with Photo Diode Array (PDA) detector. The optimal chromatographic condition was obtained using a mobile phase consisting of phosphate buffer 35mM pH 3.0: methanol (80:20), flowrate 1.0 ml/min, and 10 µl injection volume. The metamizole, thiamine and pyridoxine were detected at 275 nm and 361 nm for cyanocobalamin. The Hydrolysis of metamizole was successfully inhibited by adding solution containing 1.5 mg/mL sodium sulfite to solvent and 0.5 mg/mL sodium sulfite to mobile phase. The validation results indicate a good specificity and a linear detector responses with r>0.999. The accuracy (% recovery) for metamizole, thiamine and piridoxine were 100.26%; 99.09%; and 100.03%, respectively. The method yields good precision with RSD of metamizole, thiamine and pyridoxine were 2.0912%; 1.4489%; and 0.8418% respectively. In the robustness study, the small changes of mobile phase pH yielded unsymmetrical peaks and lower resolution. The validated method was successfully applied for simultaneous assay of metamizole, thiamine and pyridoxine in tablet. Keywords: validation; metamizole; thiamine; pyridoxine; hydrolysis of metamizole; HPLC


2021 ◽  
Vol 16 ◽  
pp. 1-9
Author(s):  
Muhammad Abdurrahman Munir ◽  
Muhammad Mukram Mohamed Mackeen ◽  
Lee Yook Heng ◽  
Khairiah Haji Badri

Histamine is a heterocyclic amine shaped by decarboxylation of the histidine. It is a compound that lack chromophore and involatile. However, the detection of histamine is imperative due to the characteristic of histamine has given several disadvantages in food industry. This paper describes methods for histamine detection by employing high performance liquid chromatography and gas chromatography. The derivatization techniques required for both methods in order to increase the sensitivity of chromatography analysis. Two derivatizing agents were applied in this study such as 9-flourenilmethyl chloroformate (FMOC – Cl) for HPLC analysis whereas for GC analysis a N,O-bis (trimethylsilyl)acetamide (BSA) was used. Method validation was in accordance to Commission Decision 657/2002/CE. The validation of specificity, linearity, precision, accuracy, detection limit and quantitation limit results indicate that the methods were acceptable. The linear range for both methods were at 0.16 – 5.00 µg∙mL-1. The determination of histamine using GC showed the superiority of this instrument compared to HPLC. Method applicability was also checked on real sample namely mackerel in order to acquire a satisfactory recovery for both methods.


2016 ◽  
Vol 11 (8) ◽  
pp. 1934578X1601100
Author(s):  
Kenny Kuchta ◽  
Jutta Ortwein ◽  
İhsan Çaliş ◽  
Rainer B. Volk ◽  
Hans W. Rauwald

Officinal European Leonurus cardiaca, East Asian L. japonicus, and South African Leonotis leonurus are traditionally used for cardiovascular, gynecological, and neurological disorders. Nevertheless, a phytochemical assessment as a basis for their quality control and comparison amongst them has not yet been reported up to now. Here, a novel RP-HPLC method is presented for quantifying twelve phenolics, lavandulifolioside, verbascoside, hyperoside, ferulic acid, isoquercitrin, rutoside, apigenin-7- O-D-glucoside, and quercitrin, as well as chlorogenic, caffeic, rosmarinic, and cichoric acids, in 18 herbal and fruit samples of the three species, as well as in a L. cardiaca refined extract. Only ferulic acid was found in every sample, whereas rosmarinic acid and apigenin-7- O-D-glucoside were not detected in any sample. Chlorogenic, caffeic, and cichoric acids and rutoside were detected in all three species. Lavandulifolioside and verbascoside, the dominant phenolics of L. cardiac, were not present in any sample of L. japonicus. Lavandulifolioside was found in this first ever HPLC analysis on phenolics of L. leonurus. Hyperoside was not found in L. cardiaca, but in both L. japonicus and L. leonurus, whereas isoquercitrin was detected in L. cardiaca and L. leonurus, but not in L. japonicus. This approach facilitates identification and quality control via HPLC/HPTLC fingerprints.


2015 ◽  
Vol 14 (1) ◽  
pp. 71-78 ◽  
Author(s):  
BK Sajeeb ◽  
Uttom Kumar ◽  
Shimul Halder ◽  
Sitesh C Bachar

Andrographis paniculata (Burm. f.) Wall. ex Nees, commonly known as Kalmegh, is widely used as antimalarial drug in herbal and traditional systems. Andrographolide is the major triterpenoid present in the plant and responsible for its therapeutic activities. The identification and quantification of andrographolide were ascertained by various spectrophotometric and chromatographic analyses. The plant sample was extracted with methanol. The amorphous residue obtained from extraction was analyzed for identification of andrographolide by chemical method, TLC, UV-Vis, FT-IR and LCMS/MS analyses. The quantitative estimation of andrographolide content in plant sample was carried out by simple reversed phase HPLC method with C18 column using a mixture of water and methanol (35:65) as mobile phase at a flow rate of 0.7 mL/min, and the estimated concentration level of andrographolide was found as 38.36±0.42 ?g/mL in the solution of amorphous residue (50 ?g/mL). After quantitative determination of andrographolide, standardization of its market preparations was accomplished using the same RP-HPLC method. The estimated % potencies of andrographolide compared to reference standard in six market preparations were found to be 97.56, 98.37, 98.21, 95.60, 98.91 and 96.40.Dhaka Univ. J. Pharm. Sci. 14(1): 71-78, 2015 (June)


1980 ◽  
Vol 63 (3) ◽  
pp. 642-646
Author(s):  
Huguette Cohen ◽  
Michel R Lapointe

Abstract A high pressure liquid chromatographic (HPLC) method is described to determine zearalenone in animal feeds at levels as low as 0.01 ppm. Samples are extracted with chloroform-ethanol and initially purified using a SEP-PAK silica cartridge, followed by column chromatography using Sephadex LH-20. Separation by normal phase HPLC is followed by fluorescence detection. Recoveries at levels of 1.0–0.01 ppm averaged greater than 90%. Confirmation included HPLC analysis of the sample and a zearalenone standard, using 3 different excitation wavelengths, and comparison of fluorescence responses obtained. The method was successfully applied to the analysis of 1 corn and 3 cornmeal samples. Zearalenone was detected in all 4 samples at levels of 0.379–19.2 ppm.


1984 ◽  
Vol 11 (1) ◽  
pp. 21-23 ◽  
Author(s):  
W. Jeffrey Hurst ◽  
Kevin P. Snyder ◽  
Robert A. Martin

Abstract An HPLC method for the determination of aflatoxins is described. The aflatoxins are extracted with aqueous acetone and interfering compounds precipitated with CuCO3. After defatting, the aflatoxins are extracted into CH2Cl2 for cleanup with silica Sep-pak® which eliminates other interfering compounds. The resulting extract is then treated with TFA to form the hemiacetal derivatives prior to final HPLC analysis. Data indicated that the method exhibits excellent accuracy and precision. In addition, it is time and solvent conservative.


2020 ◽  
Vol 5 (2) ◽  
pp. 40
Author(s):  
Mutakin Mutakin ◽  
Sandra Megantara ◽  
Batari A. Larasati ◽  
Yogiyanto Yogiyanto ◽  
Jutti Levita ◽  
...  

An HPLC method was developed and validated for the pharmacokinetic drug-drug interaction between Andrographis paniculata and ibuprofen in the plasma of Oryctolagus cuniculus rabbits after a single oral administration of the mixture. Nine healthy rabbits (6 males and 3 females, weight 1.68-2.42 kg) were acclimatized for 7 days and were randomly divided into 3 groups. At day-8th the rabbits were group (1) treated with a single oral administration of ibuprofen (dose of 28 mg/kg BW); group (2) treated with a single oral administration of Andrographis paniculata infusion (7.04 mL/kg BW); group (3) treated with a single oral administration of a mixture of Andrographis paniculata (7.04 mL/kg BW) infusion and ibuprofen (dose of 28 mg/kg BW). Plasma samples were prepared by collecting the blood from the marginal ear vein at 0, 30, 60, 90, and 120 minutes after the mixture administration, followed by centrifuging it for 30 minutes 3000 rpm. Chromatographic separation was performed on a LiChrosorb RP-18 with methanol and double-distilled water (70:30) as the mobile phase, flow rate 1 mL/minute. UV detection was set at 227 nm. The absorption and distribution of ibuprofen were fast (Tmax = 30 min; Cmax = 4.02962 mcg/mL), however, interestingly this drug could improve the absorption and distribution of andrographolide in Oryctolagus cuniculus rabbits


2020 ◽  
Vol 4 (1) ◽  
pp. 28-38
Author(s):  
Simony Martiny ◽  
Mairique Waszczuk ◽  
Samuel Kaiser ◽  
Marina Cardoso Nemitz ◽  
Valquiria Linck Bassani

The purpose of this study was to develop and validate a fast HPLC stability-indicating method for simultaneously quantifying the four main isoflavones in Trifolium pratense. Validation procedures followed the ICH requirements for complex matrices. The stability-indicating tests were performed by exposing the isoflavones to conditions of forced degradation and further analysis for verifying the formation of degradation products and their possible interferences in the HPLC analysis. The major isoflavones of Trifolium pratense proved to be stable against acid and oxidative media, thermodegradation, and photodegradation. However, they proved to be unstable in alkaline media, even for short periods of exposure like 2h. In this condition, in addition to the peaks corresponding to isoflavones, the HPLC analysis showed the presence of three additional peaks which were eluted at different retention times to the reference substances, without interfering in the quantification of the four analytes of interest, formononetin, biochanin A, daidzein and genistein. The method was validated following ICH guidelines showing to be specific, linear, precise, accurate, and robust.This first report concerning a stability-indicating method revealed that the proposed HPLC method reliably quantify the isoflavones and separate them from the degradation products in a short time of analysis.


Author(s):  
LIUDMYLA SLOBODIANIUK ◽  
LILIIA BUDNIAK ◽  
SVITLANA MARCHYSHYN ◽  
OLHA SKRYNCHUK ◽  
VICTORIIA KUDRIA

Objective: The aim of our study was to establish the content of some primary metabolites, such as amino acids in Crambe cordifolia and Crambe koktebelica. The lack of experimental data induced us to determine these compounds. Methods: Crambe cordifolia and Crambe koktebelica leaves were selected as the objects of the study. The amino acids in the raw materials were determined by the HPLC method. Results: The results of the research revealed that the leaves of Crambe cordifolia and Crambe koktebelica contain fifteen and sixteen free amino acids respectively. Among the free amino acids L-histidine was presented in Crambe cordifolia leaves in the greatest amount, its content was 12.19 µg/mg. The content of free L-arginine, L-valine, L-phenylalanine, L-isoleucine was the greatest in Crambe koktebelica leaves, it was 2.23 µg/mg, 2.04 µg/mg, 1.74 µg/mg, 1.50 µg/mg respectively. The content of bound L-glutamic acid, Glycine, L-arginine, L-leucine was the highest in Crambe cordifolia and Crambe koktebelica leaves. Conclusion: The results of the study showed that Crambe cordifolia and Crambe koktebelica can be considered as a source of highly digestible amino acids that can be used to treat some diseases.


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