scholarly journals The REVIEW ARTIKEL ANALISIS KANDUNGAN SILDENAFIL SITRAT DALAM SEDIAAN CAIR JAMU KUAT DENGAN METODE KROMATOGRAFI CAIR KINERJA TINGGI

2021 ◽  
Vol 10 (2) ◽  
pp. 13-28
Author(s):  
Fawandi Fuad Alkindi
Keyword(s):  
Formic Acid ◽  
Ammonium Acetate

Abstrak-Disfungsi ereksi merupakan masalah penting di seluruh dunia yang dialami hampir setengah dari pria diatas usia 40 tahun. Sebagian dari masyarakat Indonesia memilih untuk mengkonsumsi sediaan obat sildenafil sitrat yang dijual dipasaran untuk mengatasi disfungsi ereksi. Seiring dengan berkembangnya obat tradisional masyarakat cenderung lebih memilih mengonsumsi obat tradisional daripada obat sintetik. Obat tradisional atau yang lebih dikenal sebagai jamu yaitu bahan alam yang disediakan secara tradisional. Jamu dibuat dalam bentuk serbuk seduhan, pil, dan cairan. Jamu cair di Indonesia merupakan bentuk jamu paling disukai oleh masyarakat, dimana 59% konsumen nasional memilih jamu jenis ini. Perkembangan minat masyarakat yang besar terhadap produk jamu penambah stamina  sering disalahgunakan produsen jamu yang dalam menambahkan bahan kimia obat (BKO). Pemakaian bahan kimia obat dalam jangka panjang menyebabkan toksisitas, salah satu BKO yang sering disalahgunakan adalah sildenafil sitrat, sildenafil sitrat untuk penggunaannya harus dengan pengawasan dokter serta dalam dosis yang tepat agar tidak menimbulkan toksisitas Review artikel ini bertujuan untuk mengidentifikasi dan menjawab permasalahan pada penerapan identifikasi sildenafil sitrat pada sediaan cair jamu kuat dengan menggunakan metode KCKT. Penerapan penelitian menggunakan metode naratif dari hasil pengelompokan data-data hasil review artikel yang sejenis sesuai dengan hasil yang digunakan untuk menjawab kebutuhan metode yang akan dipakai pada penelitian. Hasil review yang diperoleh sebanyak 8 artikel yang ditemukan yaitu metode KCKT dapat digunakan untuk mengidentifikasi kandungan bahan kimia obat sildenafil sitrat dalam sediaan cair jamu kuat dengan preparasi sampel menggunakan pelarut metanol, air, dan asetonitril dan mengandung buffer asam format 0,1 % kemudian dilakukan vortex dan ultrasonik dan sistem KCKT yang digunakan yaitu  Fase gerak A (Acetonitrile):Fase gerak B (20 mmol/L ammonium acetate, 0.2% formic acid dan 10 mmol/L triethylamine) dengan elusi secara gradien Laju aliran di set 1,0 ml/menit, volume injesi 5 μL, suhu kolom diset 30˚C dan pada panjang gelombang 292 nm.

LC–MS/MS Determination of Apigenin in Rat Plasma and Application to Pharmacokinetic Study

2020 ◽  
Vol 21 ◽  
Author(s):  
Shixing Zhu ◽  
Jiayuan Zhang ◽  
Zhihua Lv ◽  
Mingming Yu
Keyword(s):  
Formic Acid ◽  
Pharmacokinetic Study ◽  
Ammonium Acetate ◽  
Rat Plasma ◽  
Biological Properties ◽  
Plasma Samples ◽  
Supply Rate ◽  
Natural Plant ◽  
Ammonium Acetate Buffer

Background: Apigenin, a natural plant flavone, has been shown to possess a variety of biological properties. Objective: In this report, a highly selective and sensitive LC-MS/MS method was developed and validated for the determination of apigenin in rat plasma. Methods: Analysts were separated on the HSS T3 column (1.8 μm 2.1×100 mm) using acetonitrile and 0.1% formic acid in 2 mM ammonium acetate buffer at a supply rate of 0.200 mL/min as eluent in gradient model. Results: Plasma samples were treated by protein precipitation using acetonitrile for the recovery ranging from 86.5% to 90.1% for apigenin. The calibration curves followed linearity in the concentration range of 0.50-500 ng/mL. The inter-day and intra-day precisions at different QC levels within 13.1% and the accuracies ranged from -10.6% to 8.6%. Conclusion: The assay has been successfully applied to the pharmacokinetic study of apigenin in rats.

scholarly journals Valorisation of Fish Bones: Effects of Preservation by Formic Acid on AL-extractable calcium, Phosphorus, Magnesium, and Potassium

2021 ◽  
Author(s):  
Anne-Kristin Løes ◽  
Johan Petter Ahlin ◽  
Ishita Ahuja ◽  
Tore Krogstad ◽  
Ståle Smevoll ◽  
...  
Keyword(s):  
Formic Acid ◽  
Laboratory Study ◽  
Gadus Morhua ◽  
Ammonium Acetate ◽  
Total Content ◽  
Water Control ◽  
Bone Material ◽  
Fish Bones ◽  
Calcium Phosphorus ◽  
Extractable Nutrients

Abstract Fishbones contain significant amounts of plant nutrients. Fish residues may be preserved by acidification to pH < 4, which may affect the extractability and plant availability of nutrients when applied as fertilisers. Grinded bone material from cod ( Gadus morhua ) heads was mixed with formic acid to investigate if acidification would increase the concentrations of ammonium acetate-lactate (AL)-extractable nutrients. Two degrees of fineness of fishbones (coarse 2-4 mm; fine < 0.71 mm) were compared at pH 3.0 and 4.0 plus a water control in a laboratory study over 55 days. Samples for extraction of AL-soluble P, Ca, Mg and K were taken on day 2, 15, 34 and 55. Whereas acidification clearly increased the concentrations of AL-extractable calcium (Ca-AL) and magnesium (Mg-AL), extractable phosphorus (P-AL) was only significantly increased in finely grinded bones at pH 3. After 34 days, 6% of the total content of P was extracted by AL in fine fishbones at pH 3. Without acidification about 1% of the P was extracted, possibly from phospholipids. This P-AL concentration was well above P-AL extracted from acidified coarse fishbones and from fine fishbones acidified to pH 4. With acidification, about 30% of total Ca and 10% of total Mg were extracted by AL, and the Ca-AL and Mg-AL concentrations were closely correlated. The reason for lower P-AL in coarse fishbones at pH 3 and 4, and fine fishbones at pH 4 than in water controls may be a precipitation of apatite from phospholipids and dissolved calcium.

Measurement of citrate in urine using liquid chromatography tandem mass spectrometry: comparison with an enzymatic method

2005 ◽  
Vol 42 (5) ◽  
pp. 357-363 ◽  
Author(s):  
BG Keevil ◽  
L Owen ◽  
S Thornton ◽  
J Kavanagh
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Formic Acid ◽  
Ammonium Acetate ◽  
Enzymatic Assay ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Urinary Citrate

Background: Measurement of urine citrate is used to assess the risk of further urinary stone formation and to assess the benefit of treatment in affected individuals. We wanted to develop a simple and rapid liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the analysis of urinary citrate and to compare it with our current enzymatic assay. Methods: For the LC-MS/MS assay, samples were prepared in a deep-well block by adding 10 µL of urine and 20 µL of internal standard to 400 µL of water. After mixing, 3 µL of the diluted sample was injected into the LC-MS/MS system. An LC system was used to isocratically elute a C18 column (50 x 2.1 mm) with 0.4 mL/min water containing 2 mmol/L ammonium acetate and 0.1% (v/v) formic acid. A step gradient of 100% methanol containing 2 mmol/L ammonium acetate and 0.1% (v/v) formic acid was used to wash the column. The retention times were 1.4 min for citrate and 1.4 min for d4-citrate. Cycle time was 4.0 min, injection to injection. The analytes were monitored using a tandem mass spectrometer operated in multiple reaction monitoring mode using the following transitions, citrate m/ z 191.0> 111.0 and d4-citrate m/ z 195.0> 113.0. Results: Within and between-batch coefficients of variation were <3% over the range 480-3800 µmol/L. The lower limit of quantification was 24.0 µmol/L. Regression analysis showed LC-MS/MS = 0.8781 (enzymatic assay) + 102.5, r = 0.964, n = 73. Conclusions: We have developed a simple LC-MS/MS method for urinary citrate measurement that shows acceptable performance.

scholarly journals DETERMINATION OF Cu(II) CONCENTRATION IN AQUEOUS MEDIUM USING INVERSION ELECTROCHEMICAL METHOD

2019 ◽  
Vol 85 (9) ◽  
pp. 58-64
Author(s):  
Vera Vorobets ◽  
Gennadii Kolbasov ◽  
Sergii Fomanyuk ◽  
Nataliia Smirnova ◽  
Oksana Linnik
Keyword(s):  
Formic Acid ◽  
Ammonium Acetate ◽  
Copper Ions ◽  
Stripping Voltammetry ◽  
Acetate Buffer ◽  
Background Solution ◽  
Ammonium Acetate Buffer ◽  
Photoelectrochemical Method ◽  
Determination Of Copper

Electrode materials based on titanium dioxide modified with zinc ions and gold nanoparticles, synthesized by sol-gel method, were used to determine the concentration of Cu (II) in liquids by stripping voltammetry method. Determination of Cu (II) was done using background solutions based on 0.4 M formic acid and ammonium acetate buffer (pH = 7.5) using the standard addition method with a potential scanning speed of 50 mV•s-1. The solution was stirred during the preliminary electrolysis at a potential of -1400 mV (vs silver-chloride reference electrode) for 120 seconds and then the potential was scanned from -1200 mV to + 200 mV. It is shown that the background solution based on ammonium acetate buffer provides a higher sensitivity and a good selectivity of peaks for the determination of copper compared to the background solution based on formic acid. Determined that value of the analytical signal of copper in the studied model solutions based on ammonium acetate and formic acid is proportional to the concentration of copper ions in the solution. To increase the selectivity of stripping voltammetry method in determining copper concentrations in solutions, an inversion spectral photoelectrochemical method was proposed, the essence of which is preliminary electroconcentration of the elements under investigation in the cathode potential region and subsequent measurement of the spectral photoelectrochemical characteristics of electroconcentration products. It has been found that in solutions of 1M ammonium acetate containing Cu2+ ions, the cathodic polarization of TiO2-based photoelectrode leads to the appearance of a cathode photocurrent and the values of photocurrent quantum yield increase with increasing content of copper ions in the solution. The spectral sensitivity of the surface layer corresponds to the absorption spectrum of Cu2O. The sensitivity of stripping voltammetry method to copper Cu (II) using the materials studied was 0.3 mg•l-1. It is shown that the inversion photoelectrochemical method is promising in the selective determination of copper concentration in liquids.

Development and validation of LC-MS/MS methods to measure tobramycin and lincomycin in plasma, microdialysis fluid and urine: application to a pilot pharmacokinetic research study

2020 ◽  
Vol 58 (2) ◽  
pp. 274-284
Author(s):  
Saurabh Pandey ◽  
Jayesh Dhanani ◽  
Jeffrey Lipman ◽  
Jason A. Roberts ◽  
Steve C. Wallis ◽  
...  
Keyword(s):  
Formic Acid ◽  
Mobile Phase ◽  
Ammonium Acetate ◽  
Research Study ◽  
Matrix Effects ◽  
Internal Standard ◽  
Gradient Elution ◽  
Acceptance Criteria ◽  
Sheep Model ◽  
Gradient Separation

AbstractBackgroundThe aim of our work was to develop and validate a hydrophilic interaction liquid chromatography-electrospray ionization-tandem mass spectrometry (HILIC-ESI-MS/MS) methods for the quantification of tobramycin (TMC) and lincomycin (LMC)in plasma, microdialysis fluid and urine.MethodsProtein precipitation was used to extract TMC and LMC from plasma, while microdialysis fluid and urine sample were diluted prior to instrumental analysis. Mobile phase A consisted of 2 mM ammonium acetate in 10% acetonitrile with 0.2% formic acid (v/v) and mobile phase B consisted of 2 mM ammonium acetate in 90% acetonitrile with 0.2% formic acid (v/v). Gradient separation (80%–10% of mobile phase B) for TMC was done using a SeQuant zic-HILIC analytical guard column. While separation of LMC was performed using gradient elution (100%–40% of mobile phase B) on a SeQuant zic-HILIC analytical column equipped with a SeQuant zic-HILIC guard column. Vancomycin (VCM) was used as an internal standard. A quadratic calibration was obtained over the concentration range for plasma of 0.1–20 mg/L for TMC and 0.05–20 mg/L for LMC, for microdialysis fluid of 0.1–20 mg/L for both TMC and LMC, and 1–100 mg/L for urine for both TMC and LMC.ResultsFor TMS and LMC, validation testing for matrix effects, precision and accuracy, specificity and stability were all within acceptance criteria of ±15%.ConclusionsThe methods described here meet validation acceptance criteria and were suitable for application in a pilot pharmacokinetic research study performed in a sheep model.

Pteridines, IXC. Synthesis, Oxidations and Reactions of 6- and 7-Hydroxy-2-thiolumazines Selective Cytotoxicity of Carboxypeptidase-activated Methotrexate ex-Peptides

Pteridines ◽  
1989 ◽  
Vol 1 (1) ◽  
pp. 57-63 ◽  
Author(s):  
Michael Bartke ◽  
Wolfgang Pfleiderer
Keyword(s):  
Elevated Temperature ◽  
Formic Acid ◽  
Nmr Spectra ◽  
Ammonium Acetate ◽  
Oxidative Desulfurization ◽  
Basic Medium ◽  
Methyl Derivative ◽  
Selective Cytotoxicity ◽  
Temperature Form ◽  
Elemental Analyses

Summary Various 6-(10, 11) and 7-hydroxy-2-thiolumazines (8,9) have been synthesized and oxidations of the thioamide function studied . H20 2 Oxidation of 7-hydroxy-2-thiolumazine (8) in basic medium leads to pteridine-4,7- dione-2-sulfinate (12), which eliminates S02 in anhydrous acids. Oxidative desulfurization of 8 and its 8- methyl derivative 9 proceeds directly in formic acid with H20 2 and m-chloroperbenzoic acid to give 16 and 17 respectively. KMn04 oxidation forms the pteridine-4,7,dione-2-sulfonates (14, 15), which react under hydrolytic conditions to give the corresponding 2-hydroxy derivtives (18, 19) and on displacement with ammonium acetate/ammonia at elevated temperature form the pterin derivatives 20 and 21.2-Thio-pteridine-4,6-dione (10) oxidizes also to the corresponding 2-sulfonate (22), which could only be isolated after addition of potassium bisulfite in the form of the dipotassium 7,8-dihydropteridine-4,6-dione- 2,7-disulfonate (23) adduct.The newly synthesized compounds have been characterized by elemental analyses, pKa determinations, UVand IH-NMR-spectra.

scholarly journals DETERMINATION OF CU(II) CONCENTRATION IN AQUEOUS MEDIUM USING INVERSION ELECTROCHEMICAL METHOD

2019 ◽  
Vol 85 (7) ◽  
pp. 24-30
Author(s):  
Vera Vorobets ◽  
Gennadii Kolbasov ◽  
Sergii Fomanyuk ◽  
Nataliia Smirnova ◽  
Oksana Linnik
Keyword(s):  
Formic Acid ◽  
Ammonium Acetate ◽  
Copper Ions ◽  
Stripping Voltammetry ◽  
Acetate Buffer ◽  
Background Solution ◽  
Ammonium Acetate Buffer ◽  
Photoelectrochemical Method ◽  
Determination Of Copper

Electrode materials based on titanium dioxide modified with zinc ions and gold nanoparticles, synthesized by sol-gel method, were used to determine the concentration of Cu (II) in liquids by stripping voltammetry method. Determination of Cu (II) was done using background solutions based on 0.4 M formic acid and ammonium acetate buffer (pH = 7.5) using the standard addition method with a potential scanning speed of 50 mV•s-1. The solution was stirred during the preliminary electrolysis at a potential of -1400 mV (vs silver-chloride reference electrode) for 120 seconds and then the potential was scanned from -1200 mV to + 200 mV. It is shown that the background solution based on ammonium acetate buffer provides a higher sensitivity and a good selectivity of peaks for the determination of copper compared to the background solution based on formic acid. Determined that value of the analytical signal of copper in the studied model solutions based on ammonium acetate and formic acid is proportional to the concentration of copper ions in the solution. To increase the selectivity of stripping voltammetry method in determining copper concentrations in solutions, an inversion spectral photoelectrochemical method was proposed, the essence of which is preliminary electroconcentration of the elements under investigation in the cathode potential region and subsequent measurement of the spectral photoelectrochemical characteristics of electroconcentration products. It has been found that in solutions of 1M ammonium acetate containing Cu2+ ions, the cathodic polarization of TiO2-based photoelectrode leads to the appearance of a cathode photocurrent and the values of photocurrent quantum yield increase with increasing content of copper ions in the solution. The spectral sensitivity of the surface layer corresponds to the absorption spectrum of Cu2O. The sensitivity of stripping voltammetry method to copper Cu (II) using the materials studied was 0.3 mg•l-1. It is shown that the inversion photoelectrochemical method is promising in the selective determination of copper concentration in liquids.

scholarly journals Quantification of plasma levels of antiviral drug sofosbuvir and its metabolite GS331007 in patients of chronic hepatitis C with chronic kidney disease using UPLC-MS/MS method

2020 ◽  
Vol 8 (1) ◽  
pp. 59-66
Author(s):  
Ruchi Singhala ◽  
Pramil Tiwaria ◽  
Ajay Dusejab ◽  
Raja Ramachandranc ◽  
Ajay Patiald ◽  
...  
Keyword(s):  
Chronic Kidney Disease ◽  
Hepatitis C ◽  
Kidney Disease ◽  
Formic Acid ◽  
Mass Spectrometer ◽  
Drug Concentration ◽  
Ammonium Acetate ◽  
Ion Trap ◽  
Hcv Infection ◽  
Linear Ion Trap

Sofosbuvir based regimens are the only treatment available in India and some other Asian countries for curing hepatitis C viral (HCV) infection. The main excretion route of sofosbuvir is renal so treatment of HCV infection is challenging in patients on hemodialysis. A simple and sensitive UPLC-MS/MS method was developed and validated according to USFDA guidelines on Linear Ion trap Quadrupole tandem mass spectrometer (QTRAP4500) which was applied to estimate the drug concentration of sofosbuvir and its metabolite GS331007 in patients of chronic kidney disease with HCV infection. Clopidogrel was used as internal standard (IS) for this study. All analytes and IS were separated on UPLC C18-HSS column (2.1mmX50mm, 1.7μm) with retention time of 2.07, 0.29 and 1.58 min, respectively, by using mobile phases of 5mM ammonium acetate in 0.2% formic acid in water (A) and 5mM ammonium acetate in 0.2% formic acid in methanol (B) on gradient elution mode at a flow rate of 0.6 mL/min. Calibration curve was plotted over the range of 10-200 μg/mL for both of the analytes and equation was calculated by applying linear regression method. Detections of daughter ions (sofosbuvir-530 to 243m/z, GS331007-261 to 112.1m/z and clopidogrel- 322 to 154.9m/z) were done in multiple reactions monitoring (MRM) mode and weights were analyzed by using Linear ion trap quadrupole mass spectrometer with turbo spray ion source. The developed method has been successfully used for quantification of drug concentration of sofosbuvir and GS331007 to see the safety of sofosbuvir in patients of HCV infection with renal failures.

scholarly journals Determination of phenolic acids and flavonoids in leaves, calyces, and fruits of Physalis angulata L. in Viet Nam

Pharmacia ◽  
2021 ◽  
Vol 68 (2) ◽  
pp. 501-509
Author(s):  
Kim-Ngan Huynh Nguyen ◽  
Ngoc-Van Thi Nguyen ◽  
Kyeong Ho Kim
Keyword(s):  
Formic Acid ◽  
Phenolic Acids ◽  
Ammonium Acetate ◽  
Gradient Elution ◽  
Viet Nam ◽  
Coumaric Acid ◽  
Aerial Parts ◽  
Physalis Angulata ◽  
Detection And Quantification

In Vietnam, Physalis angulata L. is a wild species growing throughout the country that is often used in traditional medicine. The aim of study was to quantify seven major compounds, including phenolic acids (chlorogenic acid, caffeic acid, p-coumaric acid) and flavonoids (rutin, quercitrin, quercetin, and kaempferol) in three aerial parts of P. angulata. Chromatographic separation was carried out on a Kromasil C18 column (150 mm × 4.6 mm i.d., 5 µm) with a gradient elution of 0.1% formic acid in acetonitrile, 0.2% ammonium acetate/0.1% formic acid in water and methanol at a flow rate of 1.0 mL/min; detection was at 250 and 300 nm. The limits of detection and quantification were in the ranges of 0.1–0.3 and 0.3–1.0 µg/mL, respectively. The validated method was successfully applied to analyze active compounds in P. angulata and may be a useful tool for quality control of this plant.

The structure of pre-mRNA and mRNA from erythroid cells

1978 ◽  
Vol 36 (2) ◽  
pp. 234-235
Author(s):  
A.-M. Ladhoff ◽  
B.J. Thiele ◽  
Ch. Coutelle ◽  
S. Rosenthal
Keyword(s):  
Bone Marrow ◽  
Structural Transformation ◽  
Electron Micrographs ◽  
Ammonium Acetate ◽  
Bone Marrow Cells ◽  
Erythroid Cells ◽  
Globin Mrna ◽  
Ordered Structures ◽  
Rabbit Bone ◽  
Rabbit Reticulocytes

The suggested precursor-product relationship between the nuclear pre-mRNA and the cytoplasmic mRNA has created increased interest also in the structure of these RNA species. Previously we have been published electron micrographs of individual pre-mRNA molecules from erythroid cells. An intersting observation was the appearance of a contour, probably corresponding to higher ordered structures, on one end of 10 % of the pre-mRNA molecules from erythroid rabbit bone marrow cells (Fig. 1A). A virtual similar contour was observed in molecules of 9S globin mRNA from rabbit reticulocytes (Fig. 1B). A structural transformation in a linear contour occurs if the RNA is heated for 10 min to 90°C in the presence of 80 % formamide. This structural transformation is reversible when the denatured RNA is precipitated and redissolved in 0.2 M ammonium acetate.

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