International Journal of Chemical and Analytical Science最新文献

Aims

Diclofenac sodium is a Nonsteroidal Anti-Inflammatory Drug (NSAID) with anti-inflammatory, antipyretic, and analgesic action as a result of the blockade of prostaglandin synthesis by inhibition of the cyclooxygenase enzyme. Analysis of the active pharmaceutical ingredient as well as finished pharmaceutical product is of vital importance to help ensure that good quality products are manufactured and supplied to the patient end users. The aim of the study was to develop a simple and rapid method to enable timely release of products.

Methods

The method was developed using a mobile phase prepared with environment-friendly analytical grade solvents: toluene, acetone and glacial acetic acid (10:15:0.2 v/v/v). Diclofenac sodium reference material and samples were chromatographed using pre-coated TLC silica gel 60 F₂₅₄ glass plates with a saturation time of 25 minutes and a densitometer detection wavelength of 284 nm in the reflectance absorbance mode. Detection and part of analysis was done using densitometer TLC Scanner 3 operated with Wincats (version 1.4.3) planar chromatograph software.

Results

A Thin Layer Chromatography (TLC) method for the qualitative and quantitative analysis of diclofenac sodium tablets was developed and validated according to ICH and USP guidelines. The R_f of diclofenac sodium was at 0.60 and the method was repeatable, robust with good selectivity and specificity. Regression functions were established over the range of 250–600 ng/spot with r² of 0.993 and 0.999 for the linear and polynomial regressions respectively. The accuracy at nominal concentration was found to be 100.2%, and the results of the assay of three brands for diclofenac sodium tablets were found to meet the USP 95–105% assay limits thus demonstrating the usefulness of the method for the assay of these products.

The developed assay method for diclofenac sodium in tablets is simple, accurate, and inexpensive, with good precision and should be especially useful in resource constrained countries.

Objective

To investigate antimutagenic and antioxidant potency of the aqueous heat treated Ficus benghalensis stem bark (FBH) extract and Moringa oleifera root (MRH) extract against sodium azide in TA100 tester strains of Salmonella typhimurium and their inhibition of microsomal lipid peroxidation (LPO).

Methods

Mutagenicity was assayed by the standard Ames test (standard plate incorporation assay) and antioxidant potency was investigated by employing ex vivo inhibition of lipid peroxidation in liver Microsomes.

Results

Both FBH and MRH showed strong antimutagenic effect on S. typhimurium TA100 strains against sodium azide (NaN₃). IC₅₀ values of aqueous extract of FBH and MRH extracts were 70.24 μg/ml and 99.20 μg/ml respectively. FBH extract showed maximum inhibition of microsomal lipid peroxidation responses than MRH. IC₅₀ values of aqueous extract of FBH and MRH extracts were 80.24 μg/ml and 92 μg/ml respectively. FBH and MRH exhibited a dose dependent antioxidant activity.

Conclusion

The aqueous heat-treated FBH and MRH have antimutagenic as well as antioxidant activity. Further studies are in progress to evaluate the effect of both extracts by other antioxidant and antimutagenic assays and to identify the factors responsible for these activities.

In the present paper we have reported a simple and convenient titrimetric method for determination of non-steroidal anti-inflammatory drugs (NSAIDs) e.g. aceclofenac, diclofenac sodium, ibuprofen, mefenamic acid and nimesulide in pure form and in their pharmaceutical preparations such as acecloren (Tab), aclofen (Tab), voveran (Tab), diclomax (Inj), brufen (Tab), norswell (Tab), meftal (Tab), mef-T (Tab), nicip-DT (Tab) and dolamide (Tab) with ammonium hexanitratocerate (AHC) reagent. It is a versatile oxidizing agent of cerium (IV) and is being widely used as an oxidant for several classes of organic compounds. During estimation it was noted that the excipients present in pharmaceutical preparations do not interfere. The value of percentage error, coefficient of variation (CV) and standard deviation (SD) prove the method to be precise and reproducible. To establish authenticity of the method, recovery experiments were also carried out by standard drug addition method.

Background/aim

In the present study, a series of novel phthalimide derivatives synthesized because of its potent antimicrobial and antimycobacterial activity.

Method

Structurally modified phthalimide derivatives were prepared through condensation of substituted phthalic anhydride with corresponding acetazolamide, cycloserine and isoniazid with variable yields. Synthesized Compounds (6a–d), (7a–d) and (8a–d) analyzed for their structures, in vitro antimicrobial and antimycobacterial activity.

Result

Among the synthesized compounds, compound 6b, 7b and 8b was found to be the most potent against Gram-positive bacteria Bacillus subtilis, Gram-negative bacteria Escherichia coli, Mycobacterium tuberculosis CIP and M. tuberculosis H37Rv.

Conclusion

A series of novel phthalimide derivatives of biological interest were synthesized and analyzed, suggests that it an interesting compound compared to the current therapeutic agents and are considered to investigate further for the same.

Background

Chemical diversity of endophytic fungi has made them an alternate source for bioactive compounds. Novel biotopes with promising bioactivity are expected from endophytes of medicinal plants from biodiversity hotspots. Therefore, endophytes of Nothapodytes foetida and Hypericum mysorense from Western Ghats, India were screened for free radical scavenging activity and anti-radical metabolites were profiled.

Methods

Endophytes were isolated from surface sterilized leaves, stems and barks of N. foetida and H. mysorense. Ethyl acetate extracts of culture filtrates were tested for antiradical activity using DPPH and ABTS free radicals. Antiradical spots on developed chromatogram were profiled by spraying with DPPH solution.

Results

A dose dependent antiradical activity of variable magnitude was observed. Fourteen isolates from H. mysorense and thirteen isolates from N. foetida showed significant antiradical activity. 55% of tested isolates exhibited more than 95% quenching of DPPH radicals and 40% recorded more than 75% scavenging activity. A total of 66.67% of the tested isolates recorded more than 95% scavenging of ABTS radicals and 29.6% showed more than 75% scavenging activity. TLC of active extracts showed the presence of a minimum three and maximum thirteen radical scavenging metabolite spots.

Conclusion

This is the first report on antiradical activity of endophytic isolates of H. mysorense. Active metabolite profiling would help in the further purification of most potent and abundant bioactive molecule from the fungal endophytic extracts. Further purification and characterization of the active metabolites may lead to the discovery of novel bioactive molecules of industrial and pharmaceutical importance.

Aim

The aim of the present work was to develop a novel, reliable and accurate Liquid Chromatography–Mass Spectrometry/Mass spectrometry (LC–MS/MS) method for the estimation of a potent 5-HT1B/1D receptor agonist, Rizatriptan in human plasma and to validate the proposed method.

Experimental

Zolmitriptan was used as the internal standard. The analyte and internal standard were isolated from 100 mL plasma samples by liquid-liquid extraction (LLE) and chromatographed on an ACE C18 column, (150 × 4.6 mm, 3 μm) with a mobile phase consisting of acetonitrilee10 mM aqueous ammonium acetate-acetic acid (90:10:0.5% v/v/v) pumped at 1.0 mL/min. The method had a chromatographic total run time of 10 min. A Varian 1200 L electrospray tandem mass spectrometer equipped with an electrospray ionization source was operated in multiple reaction monitoring (MRM) mode with the precursor-to-product ion transitions m/z 270.39/201.3 (Rizatriptan) and 288.43/182.2 (Zolmitriptan) used for quantitation.

Results and discussion

The method was validated over the concentration range of 50–1000 ng/ml and was found to have acceptable accuracy, precision, linearity, and selectivity. The mean extraction recovery from spiked plasma samples was above 98.26–101.32%. The intra-day accuracy of the assay ranged from 99.525 to 103.32% and intra-day precision ranged from 99.525 to 103.32% C.V. Inter-day accuracy and precision results for quality control samples ranged between 103.62 and 105.196% of nominal and precision is observed to be 5.45–10.946% C.V. The drug was found to be stable after a number of stability studies.

Conclusion

According to the validated results, the proposed method was found to be specific, accurate, and precise and could be used for the estimation of Rizatriptan in human plasma over a concentration range of 50.0–1000 ng/ml and can be applied for the routine analysis.

Context

Micellar thin layer chromatography (MLC) used for separation of various heavy metal ions from various environmental samples. MLC successfully applied for semiquanitative and spectrometry identification of metal ions.

Objective

Utilization of MLC in separation, semiquanitative determination and Chromatospectrometric method for estimation of ${\text{UO}}_2^{2+}$ on bismuth silicate layer, using Tween-80.

Method

Ascending development of the plates performed with aq. micellar, hydro-organic and water-organic-surfactant as mobile phase. Separation carried out on thin layer of bismuth silicate and layer developed with non-ionic surfactant Tween-80.

Results and conclusions

Acetone was found to be most effective additive at 10% concentration with 5% Tween-80. This method successfully applied to identification and separation of Cd₂, Hg₂ and Co₂ from river water and industrial wastewater. Semiquantitative as well as spectrometry techniques was used for quantitative analysis of ${\text{UO}}_2^{2+}$ in river water with preliminary separation from Fe₃ and Cu₂. Maximal recovery of 90% observed. This TLC method is rapid, with development times averaging 2–5 min.