Validasi Metode Analisis Kapsul Rifampisin Dengan HPLC-PDA

Andi Suhendi; Erlya Ayusari Ramly

doi:10.22236/farmasains.v8i1.5602

Validasi Metode Analisis Kapsul Rifampisin Dengan HPLC-PDA

Farmasains : Jurnal Ilmiah Ilmu Kefarmasian ◽

10.22236/farmasains.v8i1.5602 ◽

2021 ◽

Vol 8 (1) ◽

pp. 31-36

Author(s):

Andi Suhendi ◽

Erlya Ayusari Ramly

Keyword(s):

Ammonium Hydroxide

Rifampisin merupakan salah satu obat anti-tuberkulosis. HPLC merupakan metode pilihan karena kepekaan, reprodusibilitas dan spesifitasnya. Namun metode terbaru dari kromatografi cair membutuhkan penambahan tetra-butyl ammonium hydroxide yang dapat memperpendek umur kolom. Penelitian ini bertujuan untuk mengembangkan suatu metode kromatografi cair dengan waktu pengerjaan yang efisien dibandingkan metode-metode sebelumnya. Sistem kromatografi yaitu HPLC Alliance 2695, C18 (100 x 4,6 mm; 5 µm), fase gerak sistem gradient berupa asetonitril dan akuades dengan laju alir 1,0 mL/menit dan dideteksi pada 254 nm. Hasil penetapan parameter validasi didapatkan bahwa metode akurat dengan %recovery 99,96 ± 0,04% dan RSD 0,64 ± 0,30%. Parameter linieritas didapatkan koefisien korelasi 0,998, kerberulangan dan presisi antara didapatkan RSD masing-masing yaitu 1,51% dan 1,54%. Nilai LoQ didapatkan dari persamaan regresi linier residual yaitu 0,0164%. Metode yang divalidasi memenuhi parameter validasi akurasi, presisi dan linieritas.

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Fine MCP Decapsulation Technology Development

ISTFA 2006: Conference Proceedings from the 32nd International Symposium for Testing and Failure Analysis ◽

10.31399/asm.cp.istfa2006p0474 ◽

2006 ◽

Author(s):

Jianwei Zhou ◽

Wei Zheng ◽

Taekoo Lee

Keyword(s):

Chemical Etching ◽

Etch Rate ◽

Technology Development ◽

New Technology ◽

Ammonium Hydroxide ◽

Mechanical Polishing ◽

Technology Process ◽

Tetra Methyl Ammonium Hydroxide ◽

Die Surface

Abstract Multi-Chip Package (MCP) decapsulation is now becoming a rising problem. Because for traditional decapsulation method, acid can’t dissolve the top silicon die to expose the bottom die surface in MCP. It makes inspecting the bottom die in MCP is difficult. In this paper, a new MCP decapsulation technology combining mechanical polishing with chemical etching is introduced. This new technology can remove the top die quickly without damaging the bottom die using KOH and Tetra-Methyl Ammonium Hydroxide (TMAH). The technology process and relative application are presented. The factors that affect the KOH and TMAH etch rate are studied. The usage difference between the two etchant is discussed.

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Development and Validation of Stability Indicating HPLC Method for the Determination of Impurities in the Sterile Mixture of Cefoperazone and Sulbactam

Current Pharmaceutical Analysis ◽

10.2174/1573412914666180914163419 ◽

2019 ◽

Vol 15 (7) ◽

pp. 762-775

Author(s):

Ramu Ivaturi ◽

Thuttagunta Manikya Sastry ◽

Satyaveni Sunkara

Keyword(s):

Quantitative Estimation ◽

Ammonium Hydroxide ◽

Hplc Method ◽

Forced Degradation ◽

Buffer Solution ◽

Solution Ph ◽

Pharmaceutical Dosage Forms ◽

Stability Indicating ◽

Validation Parameters ◽

Abdominal Infections

Background: Cefoperazone Sulbactam injection is a cephalosporin antibiotic with a β- lactamase inhibitor used in the treatment for intra abdominal infections, Urinary track infections, surgical infections, etc. The combination is not official in any of the pharmacopeia for their content and impurities determination. Introduction: The present study involves the development of a simple, rapid, accurate, sensitive and stability indicating RP-HPLC method for the quantitative estimation of Cefoperazone Sulbactam mixture and its impurities in bulk and pharmaceutical dosage forms. Methods: 0.005 M Tetrabutyl ammonium hydroxide buffer solution pH adjusted to 6.80 and Acetonitrile combination has been used in a gradient programme with a flow rate of 1.0 ml/min. The retention time of Cefoperazone and Sulbactam were observed at around 8.5 and 19.5 minutes respectively. The UV detection was carried out at a wavelength of 230 nm. The chromatographic separation was achieved using Waters xbridge C18-150*4.6 mm, 3.5 µm HPLC column. The method has been validated according to the current International Council for Harmonization (ICH) guidelines for the method validation parameters such as Specificity, linearity, range, accuracy, precision, robustness and sensitivity. Results: The validation results indicate that the method is specific, as the known impurities and other impurities formed during the forced degradation studies were not co-eluting with the main components. Moreover, all these impurities were found to be spectrally pure, proving the stability indicating power of the method. The linearity and range of the method is in the range of 0.01-150%, highly accurate (100.2%), precise (<1%) and robust. Conclusion: The proposed method was accurate and specific for the quantitative analysis of Cefoperazone and Sulbactam and their related impurities in the sterile mixture. Hence the proposed method can be used for the quantification of impurities in routine as well as stability analysis in the development as well as quality control laboratories.

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Ozone and Ammonium Hydroxide Modification of Biochar Prepared from Pisum sativum Peels Improves the Adsorption of Copper (II) from an Aqueous Medium

Environmental Processes ◽

10.1007/s40710-020-00455-2 ◽

2020 ◽

Vol 7 (3) ◽

pp. 973-1007

Author(s):

Mohamed A. El-Nemr ◽

Nabil M. Abdelmonem ◽

Ibrahim M. A. Ismail ◽

Safaa Ragab ◽

Ahmed El Nemr

Keyword(s):

Pisum Sativum ◽

Aqueous Medium ◽

Ammonium Hydroxide

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Investigating the Effects of Surface Adsorbates on Gold and Palladium Deposition on Carbon

Topics in Catalysis ◽

10.1007/s11244-021-01423-2 ◽

2021 ◽

Author(s):

Bethany Bowden ◽

Josh A. Davies-Jones ◽

Matthew Davies ◽

Philip R. Davies ◽

David J. Morgan ◽

...

Keyword(s):

Aqueous Solutions ◽

Ammonium Hydroxide ◽

Ammonium Ion ◽

Metallic State ◽

Chloroauric Acid ◽

Final State ◽

Ammonium Thiosulfate ◽

Surface Adsorbates ◽

Surface Hydroxyls ◽

High Concentrations

AbstractSurface functional groups have a strong influence on the deposition and final state of nanoparticles adsorbed on to the surface, a role discussed by Professor Spencer in his work. This tribute to Spencer explores the formation of hydroxyls, thiosulfates, sulfites and sulfur atoms on carbon (HOPG) surfaces and their effect on the deposition of gold and palladium from aqueous solutions. Hydroxyls formed from ammonium hydroxide treatment have identical behaviour to those formed by acid treatment, and gold adsorption from Au3+ solutions gives Au0 initially, with Au3+ formed at higher concentrations on these surfaces. In contrast, palladium adsorption is hindered by the presence of the hydroxyls and there is no indication of any reduction to the metallic state. Ammonium thiosulfate adsorbs dissociatively from aqueous solutions on HOPG if the surface is pre-activated by the presence of surface hydroxyls. At low concentrations of ammonium thiosulfate, adsorbed sulfite and sulfur are formed in equimolar concentrations whereas adsorption of high concentrations of ammonium thiosulfate gives some degree of molecular adsorption, with evidence in XP spectra for an ammonium ion and a sulfur 2p peak at 282.9 eV attributed to the undissociated thiosulfate ion. Both sulfur and the sulfite are stable at the surface in neutral solutions but the sulfite desorbs when treated with acidified solutions (~ pH ≤ 6). These two groups are also stable at 373 K but begin to desorb by 473 K. Exposure to a weak chloroauric acid solution causes the desorption of the sulfite and formation of a gold species with an XP binding energy of 84.6 eV; we cannot determine from the present data whether this peak is due to a Au(I) state or very small nanoparticles of Au(0). Graphic Abstract

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Grafting of (3-Chloropropyl)-Trimethoxy Silane on Halloysite Nanotubes Surface

Applied Sciences ◽

10.3390/app11125534 ◽

2021 ◽

Vol 11 (12) ◽

pp. 5534

Author(s):

Asmaa M. Abu El-Soad ◽

Giuseppe Lazzara ◽

Alexander V. Pestov ◽

Daria P. Tambasova ◽

Denis O. Antonov ◽

...

Keyword(s):

Active Site ◽

Chemical Engineering ◽

Coupling Reaction ◽

Ammonium Hydroxide ◽

Halloysite Nanotubes ◽

Chemical Activity ◽

Molar Ratio ◽

New Materials ◽

Experimental Conditions ◽

Trimethoxy Silane

Modified halloysite nanotubes (HNTs-Cl) were synthesized by a coupling reaction with (3-chloropropyl) trimethoxysilane (CPTMS). The incorporation of chloro-silane onto HNTs surface creates HNTs-Cl, which has great chemical activity and is considered a good candidate as an active site that reacts with other active molecules in order to create new materials with great applications in chemical engineering and nanotechnology. The value of this work lies in the fact that improving the degree of grafting of chloro-silane onto the HNT’s surface has been accomplished by incorporation of HNTs with CPTMS under different experimental conditions. Many parameters, such as the dispersing media, the molar ratio of HNTs/CPTMS/H2O, refluxing time, and the type of catalyst were studied. The greatest degree of grafting was accomplished by using toluene as a medium for the grafting process, with a molar ratio of HNTs/CPTMS/H2O of 1:1:3, and a refluxing time of 4 h. The addition of 7.169 mmol of triethylamine (Et3N) and 25.97 mmol of ammonium hydroxide (NH4OH) led to an increase in the degree of grafting of CPTMS onto the HNT’s surface.

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Fluorometric Determination of Chlortetracycline in Mixed Feeds

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/47.2.203 ◽

1964 ◽

Vol 47 (2) ◽

pp. 203-208

Author(s):

Stanley E Katz ◽

Joseph Spock

Keyword(s):

Ion Exchange ◽

Exchange Resin ◽

Ammonium Hydroxide ◽

Solvent System ◽

Ion Exchange Resin ◽

Alkaline Degradation ◽

Fluorometric Determination ◽

Mixed Feeds ◽

Microbiological Assays

Abstract The fluorometric procedure for chlortetracycline in mixed feeds is based upon the degradation of chlortetracycline in alkaline solution to isochlortetracycline. The fluorescence of the isochlortetracycline is directly proportional to the concentration of chlortetracycline present prior to alkaline degradation. Chlortetracycline is extracted from mixed feeds with an acidmethanol solvent system, separated from the feed extract by adsorption on a Dowex 50 ion exchange resin, and eluted from the resin by ammonium hydroxide after conversion to isochlortetracycline. The isochlortetracycline is measured fluorometrically. Recoveries from known feeds are generally greater than 90% and agreements with microbiological assays are very close.

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