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1

Development and validation of HPLC-UV method for the quantitative analysis of carcinogenic organic impurities and its isomers in the sodium polystyrene sulfonate polymer

Zinjad Pushpavati, Gondhale Priyanka, Kulkarni Shrikant, Musmade Bhaskar, Bhope Shrinivas, Padmanabhan Sriram

Acta Chromatographica

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2021

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Vol. 33, no. 2

162--169

EN

Sodium polystyrene sulfonate (SPS) powder is in use for over 50 years for the treatment of hyperkalemia. SPS powder is official in United States Pharmacopoeia, British Pharmacopoeia and European Pharmacopoeia. However, till date, no study has been published on the assessment of organic impurities for this drug. The organic impurities in bulk drug and finished product are associated with their safety, efficacy and stability. A simple, rapid, specific, precise and an accurate HPLC method has been developed for the estimation of toxic organic impurities like styrene, naphthalene, divinyl benzene (DVB) and ethylvinyl benzene (EVB) from SPS bulk drug and finished product. The developed method was validated for specificity, accuracy, precision, linearity, limit of detection (LOD), limit of quantitation (LOQ), solution stability, ruggedness and robustness. The influence of acid, alkali, oxidative stress, photolytic stress, thermal stress and humidity stress conditions on SPS bulk powder and finished product has been studied and reported. The proposed method can be successfully employed for the impurity testing of commercial batches of the bulk drug and finished products of both sodium salt and calcium salt of polystyrene sulfonate.

2

A reliable HPLC-DAD method for simultaneous determination of related substances in TBI-166 active pharmaceutical ingredient

Zhang Tingting, Yin Wanting, Jin Bo, Li Tong, Ma Chen

Acta Chromatographica

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2020

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Vol. 32, no. 2

80--85

EN

A sensitive, stability-indicating reversed-phase high-performance liquid chromatography with diode array detection (HPLC–DAD) method has been developed for the determination of TBI-166 and its 10 kinds of related impurities. Chromatographic separation was achieved on a Kromasil ODS column (250 mm × 4.6 mm, 5 μm), with a gradient elution of the mobile phase system consisting of acetonitrile and 1% ammonium formate solution (with 0.2% formic acid). The flow rate was 1.0 mL/min, and the detection wavelength was set at 251 nm. The method was validated according to the International Conference on Harmonization (ICH) guidelines with respect to selectivity, linearity, limits, accuracy, precision, and robustness. The calibration curves were linear from LOQ to 150% of the specification limit of impurity with correlation coefficients not less than 0.999. The limits of quantitation were between 0.123 and 0.257 μg/mL. Accuracy for the related substances was estimated by the recovery ranged from 94.6% to 111.2%. The method was proved to be reliable for the determination of related substances in TBI-166 bulk drug, which is essential and important in the quality control.

3

Validated Selective HPLC-DAD Method for the Simultaneous Determination of Diclofenac Sodium and Lidocaine Hydrochloride in Presence of Four of Their Related Substances and Potential Impurities

Belal T. S., Bedair M. M., Gazy A. A., Guirguis K. M.

Acta Chromatographica

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2015

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Vol. 27, no. 3

477--493

EN

This study presents a selective high-performance liquid chromatography (HPLC) with diode array detection (DAD) method for the simultaneous estimation of diclofenac sodium and lidocaine hydrochloride in presence of four of their related substances and potential impurities, namely, 2,6-dimethylaniline (DMA), 2,6-dichloroaniline (DCA), N-phenyl-2,6-dichloroaniline (PDCA), and N-chloroacetyl-N-phenyl-2,6-dichloroaniline (CPDCA). Some of these related substances are reported as degradation products as well. Effective chromatographic separation was achieved using Waters Symmetry C18 column, (3.9 × 150 mm, 5 μm particle size) with gradient elution of the mobile phase composed of 0.05 M orthophosphoric acid and acetonitrile. The gradient elution started with 5% (by volume) acetonitrile, ramped up linearly to 65% in 5 min then kept constant till the end of the run. The mobile phase was pumped at a flow rate of 1.5 mL min−1. The multiple wavelength detector was set at 220 nm, and quantification of both drugs was based on measuring their peak areas. The retention times for lidocaine and diclofenac were about 5.5 and 9.5 min, respectively. The reliability and analytical performance of the proposed HPLC procedure were statistically validated with respect to system suitability, linearity, ranges, precision, accuracy, specificity, robustness, detection, and quantification limits. Calibration curves were linear in the ranges of 10–200 μg mL−1 for both drugs with correlation coefficients not less than 0.9998. The proposed method proved to be selective by resolution of the two drugs from their related substances and potential impurities. The validated HPLC method was successfully applied to the analysis of this binary mixture in the combined formulation (ampoules dosage form), and the assay results were favorably compared with a previously reported HPLC method. The proposed method made use of DAD as a tool for peak identity and purity confirmation.

4

Determination of spectinomycin and related substances by HPLC coupled with evaporative light scattering detection

Wang Y, Wang M. J, Li J., Yao S. C, Xue J, Zou W. B, Hu C.

Acta Chromatographica

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2015

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Vol. 27, no. 1

93--109

EN

An improved ion-pairing reversed-phase high-performance liquid chromatography method coupled with evaporative light scattering detection (HPLC-ELSD) was developed to determine spectinomycin and its related substances in commercial samples. The method was validated in accordance with International Conference on Harmonization (ICH) guidelines. The specificity of the HPLC-ELSD method was similar to that of the European Pharmacopoeia (Ph. Eur.) method, and repeatability and robustness were markedly improved relative to other reported methods due to our empirical evaluation of separation columns. Indeed, it is a more specific assay of spectinomycin than traditional microbiological techniques. The HPLC-ELSD method was used to evaluate the impurity profiles of eight compounds in seven spectinomycin batches from five different companies. Liquid chromatography coupled with electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) was employed to characterize the structures of these compounds. Though the HPLC-ELSD method was not as sensitive as the Ph. Eur. method, its limit of quantitation (LOQ) (0.16%) was lower than the disregard limit (0.3%) described by the Ph. Eur. 7.0. This suggests that the HPLC-ELSD method is appropriate for routine analysis of spectinomycin and its related substances.

5

Development and application of stability-indicating HPLC method for the determination of nevirapine and its impurity in combination drug product

Navaneethan G, Karunakaran K., Elango K. P

Acta Chromatographica

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2012

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Vol. 24, no. 4

575--587

EN

A stability-indicating reversed-phase high-performance liquid chromatography method has been developed and validated for the estimation of nevirapine and its impurity, namely the related compound A and the related compound B in combination drug product. The separation was carried out on SUPELCOSIL ABZ (150 mm × 4.6 mm, 5 µm) column. Tablet was admitted to the stress conditions of acid, base, peroxide, thermal, humidity, and photolytic degradation. The degradation products were well resolved from nevirapine, and its impurities peaks and the peak homogeneity of compound were obtained using photo diode array detector, hence proving the stability-indicating nature of the method. Moreover, to prove the selectivity of the method, individual lamivudine, zidovudine, and their main impurities were injected. The developed method was linear for nevirapine from 120 to 360 µg mL-1, and the linear regression obtained was >0.999. Recovery data were in the range 98.2–101.5%. The limit of quantification for related compound A and related compound B was found to be 0.02%. The proposed method was validated according to the International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use guidelines and proved suitable for stability testing and quality control of these drugs in pharmaceutical preparations.

6

Metale i substancje towarzyszące w wodzie do picia u konsumentów w Poznaniu

Górski J., Siepak M.

Biuletyn Państwowego Instytutu Geologicznego

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2011

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nr 445 Hydrogeologia z. 12/1

139--148

PL

W pracy przedstawiono wyniki oznaczeń glinu, arsenu, kadmu, miedzi, ołowiu, cynku, niklu, żelaza, manganu oraz wapnia, magnezu, sodu, chlorków, siarczanów, azotanów, pH, przewodności elektrolitycznej właściwej i zasadowości w próbkach wody pobranych bezpośrednio u konsumentów z sieci wodociągowej miasta Poznania. Próbki wody pobierano w maju 2010 roku, w strefie zaopatrzenia miasta w wodę do picia z ujęcia Dębina, zasilanego ze sztucznej infiltracji. Łącznie do analizy fizyczno-chemicznej pobrano 100 próbek wody oraz dodatkowo 10 próbek dublowanych i 10 próbek ślepych terenowych w celu kontroli jakości QA/AC. Oznaczeń pierwiastków dokonano przy wykorzystaniu spektrometru masowego z jonizacją w plazmie indukcyjnie sprzężonej (ICP-MS), optycznego spektrometru emisyjnego ze wzbudzeniem w plazmie indukcyjnie sprzężonej (ICP-OES) oraz wysokosprawnej chromatografii jonowej (HPIC). W wodzie uzdatnionej z ujęcia Dębina nie stwierdzono przekroczeń dopuszczalnych stężeń badanych metali. W wodzie do picia u konsumentów stwierdzono wzrost stężeń maksymalnych dla większości badanych metali, w wyniku ich ługowania z sieci i armatury wodociągowej. W przypadku kadmu, miedzi, niklu, ołowiu i manganu stwierdzono przekroczenia dopuszczalnych stężeń. Przeanalizowano wpływ różnych czynników na występowanie podwyższonych stężeń metali w wodzie wodociągowej.

EN

The paper presents the results of determinations of aluminum, arsenic, cadmium, copper, lead, zinc, nickel, iron, manganese, calcium, magnesium, sodium, chlorides, sulphates, nitrates, pH, electrolytic conductivity and alkalinity in water samples collected directly at consumers from the water pipe network in the city of Poznań. The water samples were collected in May 2010 in the drinking water supply zone from the Dębina well-field. The total number of 100 water samples and, additionally, 10 doubled samples and 10 zero samples to ensure QA/AC were collected for physicochemical analysis. The determinations of the investigated elements were performed using an inductively coupled plasma mass spectrometer (ICP-MS), an inductively coupled plasma optical emission spectrometer (ICP-OES) and high-performance ion chromatography (HPIC). The allowable concentrations of the metals in the treated water from the Dębina well-field were not exceeded. The water collected at consumers shows the increase in the maximum concentrations for most investigated metals as a result of their leaching from the water pipe network and fittings. In the case of cadmium, copper, nickel, lead and manganese, the allowable concentrations were exceeded – in four samples for nickel and in single samples for the other metals. The influence of various factors on the occurrence of increased metal concentrations in piped water at consumers was also analysed.