A new issue of this journal has just been published. To see abstracts of the papers it contains (with links through to the full papers) click here:
Selected papers from the latest issue:
Simultaneous quantification of L- α -phosphatidylcoline and cholesterol in liposomes using near infrared spectrometry and chemometry
01 February 2012, 02:49:58
Publication year: 2012
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 31 January 2012
Alina Porfire, Ioan Tomuta, Lucia Tefas, Sorin E. Leucuta, Marcela Achim
This paper describes the development and validation of a multivariate method based on transmittance NIR spectroscopy for simultaneous quantification of L- α–phosphatidylcoline (LPC) and cholesterol (CHO). Method development was based on a D-optimal experimental design consisting of 16 LPC-CHO mixtures. Calibration models were generated by partial least-squares (PLS) and principal component regression (PCR) method followed by leave-one-out cross-validation. Among the spectra pretreatment methods tested, Norris Gap first derivative was the best for both LPC and CHO quantification, combined with PLS multivariate method. The method was validated (trueness, precision, accuracy) for the concentration range 50-150% of the expected concentration in liposomes. This method was successfully applied for the characterization of liposomes prepared using the two excipients.
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 31 January 2012
Alina Porfire, Ioan Tomuta, Lucia Tefas, Sorin E. Leucuta, Marcela Achim
This paper describes the development and validation of a multivariate method based on transmittance NIR spectroscopy for simultaneous quantification of L- α–phosphatidylcoline (LPC) and cholesterol (CHO). Method development was based on a D-optimal experimental design consisting of 16 LPC-CHO mixtures. Calibration models were generated by partial least-squares (PLS) and principal component regression (PCR) method followed by leave-one-out cross-validation. Among the spectra pretreatment methods tested, Norris Gap first derivative was the best for both LPC and CHO quantification, combined with PLS multivariate method. The method was validated (trueness, precision, accuracy) for the concentration range 50-150% of the expected concentration in liposomes. This method was successfully applied for the characterization of liposomes prepared using the two excipients.
Highlights
► L-α–phosphatidylcholine (LPC) quantification by NIR spectroscopy ► Cholesterol (CHO) quantification by NIR spectroscopy ► PLS multivariate method for LPC and CHO quantification ► Method validation by trueness, precision, accuracy, uncertaintyThe paradigm shifting role of chromatographic methods in pharmaceutical analysis
30 January 2012, 23:16:24
Publication year: 2012
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 30 January 2012
Sándor Görög
An overview is presented of the impact of chromatographic method developments on the quality control of pharmaceuticals as of the 1950s up until the present times. This survey is mainly based on the changes in pharmacopoeias starting with United States Pharmacopoeia (USP) 16, issued in 1960, up to the presently effective USP 34 and European Pharmacopoeia 7.2. At the beginning of this period the role of chromatographic methods was negligible and was restricted to classical column chromatography and paper chromatography. However, the invention of high-performance liquid chromatography (HPLC) initiated a rapid paradigm shift in the attitude towards, and the use of, chromatographic methods. As a result, HPLC began a “career” of rapid spreading and development, and by now has undoubtedly become the principal method in pharmaceutical analysis. Likewise, the role of thin-layer chromatography (TLC) and to a lesser extent gas chromatography is also remarkable. The role of these and electrophoretic methods in the identification, assay and purity check of drugs and drug products in the modern pharmacopoeias is discussed.As a case study the stability investigation of Depersoloneinjection carried out in the 1960s and 35 years later is presented and the information obtainable from the classical and modern approach is compared.
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 30 January 2012
Sándor Görög
An overview is presented of the impact of chromatographic method developments on the quality control of pharmaceuticals as of the 1950s up until the present times. This survey is mainly based on the changes in pharmacopoeias starting with United States Pharmacopoeia (USP) 16, issued in 1960, up to the presently effective USP 34 and European Pharmacopoeia 7.2. At the beginning of this period the role of chromatographic methods was negligible and was restricted to classical column chromatography and paper chromatography. However, the invention of high-performance liquid chromatography (HPLC) initiated a rapid paradigm shift in the attitude towards, and the use of, chromatographic methods. As a result, HPLC began a “career” of rapid spreading and development, and by now has undoubtedly become the principal method in pharmaceutical analysis. Likewise, the role of thin-layer chromatography (TLC) and to a lesser extent gas chromatography is also remarkable. The role of these and electrophoretic methods in the identification, assay and purity check of drugs and drug products in the modern pharmacopoeias is discussed.As a case study the stability investigation of Depersoloneinjection carried out in the 1960s and 35 years later is presented and the information obtainable from the classical and modern approach is compared.
Highlights
► The role of chromatographic methods in pharmacopoeias in 1960 and at present. ► The role of chromatographic methods in contemporary pharmaceutical analysis. ► Case study demonstrating the changes in drug analysis in the last half century.Development of a method for the determination of 4-(Methylnitrosamino)-1-(3-pyridyl)-1-butanol in urine of nonsmokers and smokers using liquid chromatography/tandem mass spectrometry
30 January 2012, 23:16:24
Publication year: 2012
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 29 January 2012
Hou Hongwei, Zhang Xiaotao, Tian Yongfeng, Tang Gangling, Liu Yulan, ...
4-(Methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL) is an efficient biomarker of tobacco-specific carcinogen 4-(Methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK). The ability to monitor biomarker concentrations is very important in understanding potential cancer risk. An analytical method using molecularly imprinted polymer (MIP) column coupled with liquid chromatography/tandem mass spectrometry (LC-MS/MS) for the determination of total NNAL in human urine was developed and validated. The combination of MIP column extraction and LC-MS/MS can provide a high sensitive and relatively simple analytical method. The limit of detection (LOD) was 0.30 pg/ml and analysis time was 6 min. The method has been applied to urine samples of 36 nonsmokers and 207 smokers. NNAL was found to be significantly higher in the urine of smokers compared with nonsmokers. Compared with smokers with blended cigarettes, chinese virginia cigarettes smokers had low urinary NNAL levels. There was a direct association between the 24-hour mouth-level exposure of carcinogen NNK from cigarette smoking and the concentration of NNAL in the urine of smokers. However, there was not a positive correlation between urinary total NNAL levels in 24 h and tar. Total urinary NNAL is a valuable biomarker for monitoring exposure to carcinogenic NNK in smokers and in nonsmokers. A prediction model of cigarette smoke NNK and urinary average NNAL levels in 24 h was established (y = 2.8987x-245.38,r = 0.9952, n = 204).
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 29 January 2012
Hou Hongwei, Zhang Xiaotao, Tian Yongfeng, Tang Gangling, Liu Yulan, ...
4-(Methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL) is an efficient biomarker of tobacco-specific carcinogen 4-(Methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK). The ability to monitor biomarker concentrations is very important in understanding potential cancer risk. An analytical method using molecularly imprinted polymer (MIP) column coupled with liquid chromatography/tandem mass spectrometry (LC-MS/MS) for the determination of total NNAL in human urine was developed and validated. The combination of MIP column extraction and LC-MS/MS can provide a high sensitive and relatively simple analytical method. The limit of detection (LOD) was 0.30 pg/ml and analysis time was 6 min. The method has been applied to urine samples of 36 nonsmokers and 207 smokers. NNAL was found to be significantly higher in the urine of smokers compared with nonsmokers. Compared with smokers with blended cigarettes, chinese virginia cigarettes smokers had low urinary NNAL levels. There was a direct association between the 24-hour mouth-level exposure of carcinogen NNK from cigarette smoking and the concentration of NNAL in the urine of smokers. However, there was not a positive correlation between urinary total NNAL levels in 24 h and tar. Total urinary NNAL is a valuable biomarker for monitoring exposure to carcinogenic NNK in smokers and in nonsmokers. A prediction model of cigarette smoke NNK and urinary average NNAL levels in 24 h was established (y = 2.8987x-245.38,r = 0.9952, n = 204).
Highlights
► NNAL was analyzed by molecularly imprinted polymer column coupled with LC-MS/MS ► The LOD was 0.30 pg/ml and analysis time was 6 min Urine samples of 36 nonsmokers and 207 smokers were applied ► There was not a positive correlation between urinary NNAL levels in 24 h and tar ► There was a direct association between the NNK and NNAL ► A prediction model of NNK and urinary average NNAL levels in 24 h was established.Identification of phenolic compounds fromScutellaria laterifloraby liquid chromatography with ultraviolet photodiode array and electrospray ionization tandem mass spectrometry
30 January 2012, 23:16:24
Publication year: 2012
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 29 January 2012
Jing Li, Yan-Hong Wang, Troy J. Smillie, Ikhlas A. Khan
Scutellaria lateriflora(American skullcap) has been used more than 200 years as a mild relaxant and as a therapy for anxiety, nervous tension, and convulsions. Currently, it is one of the most popular botanicals with many products on the USA market. Flavonoids with anxiolytic property have been reported from the aerial parts of this plant. From the HPLC chromatogram of the methanolic extract of this plant, it can be concluded that some flavonoids have not been identified yet. In the present study a simple high-performance liquid chromatography with UV and electrospray ionization mass spectrometric detection (HPLC-DAD/ESI-MS) method has been developed for the identification of major phenolic compounds from it. The ESI-MSfragmentation pathways of four types of flavonoid references have been interpreted which provide very useful guidance for the characterization of different types of flavonoids from this plant. Further analysis of the methanolic extract of American skullcap based on the combination of their fragmentation patterns with the UV spectra led to characterize thirteen flavonoids and one stilbene derivative, seven of which are described for the first time from this species.
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 29 January 2012
Jing Li, Yan-Hong Wang, Troy J. Smillie, Ikhlas A. Khan
Scutellaria lateriflora(American skullcap) has been used more than 200 years as a mild relaxant and as a therapy for anxiety, nervous tension, and convulsions. Currently, it is one of the most popular botanicals with many products on the USA market. Flavonoids with anxiolytic property have been reported from the aerial parts of this plant. From the HPLC chromatogram of the methanolic extract of this plant, it can be concluded that some flavonoids have not been identified yet. In the present study a simple high-performance liquid chromatography with UV and electrospray ionization mass spectrometric detection (HPLC-DAD/ESI-MS) method has been developed for the identification of major phenolic compounds from it. The ESI-MSfragmentation pathways of four types of flavonoid references have been interpreted which provide very useful guidance for the characterization of different types of flavonoids from this plant. Further analysis of the methanolic extract of American skullcap based on the combination of their fragmentation patterns with the UV spectra led to characterize thirteen flavonoids and one stilbene derivative, seven of which are described for the first time from this species.
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