Enantioselective HPLC analysis of escitalopram oxalate and its impurities using a cellulose-based chiral stationary phase under normal- and green reversed-phase conditions.

Normal-phase and reversed-phase high-performance liquid chromatography methods for the separation of the active pharmaceutical ingredient escitalopram from its (R)-enantiomer impurity have been developed on the cellulose-based Chiralcel OJ-H chiral stationary phase. Both methods share two features: they use ethanol as a cosolvent and are able to give a complete enantioseparation without interference from other associated chiral impurities. With the green eluent mixture ethanol-water-diethylammine 70:30:0.1 (v/v/v), the resolution between escitalopram and (R)-enantiomer was 2.09 at 30°C. The limits of quantification for the (S) and (R) enantiomers were 4.5 and 3.8 µg mL-1 , respectively.

A case of medicine in disguise: motion sickness patches sold as medical devices containing active pharmaceutical substances.

INTRODUCTION: A case study is reported on anti-motion sickness transdermal patches sold in the Internet, claiming to contain only natural ingredients but, actually, containing undeclared medicinal active substances. The visual inspection of the samples evidenced many inconsistencies in secondary and primary packaging, missing of various legal information and a non-compliant "CE" mark. METHODS: The qualitative analysis was performed by liquid chromatography - high resolution mass spectrometry and the quantitative by liquid chromatography with diode array detector. RESULTS: The analyses evidenced the presence of the antihistaminic drug Diphenhydramine and of other active substances (Capsaicin, a transdermal absorption enhancer, and Diclofenac in traces, probably a contaminant from other productions of the same plant). Moreover, the presence of several trace elements, including those potentially toxic to humans, was assessed by ICP-MS analysis. CONCLUSIONS: The case discussed is a new case of "medicines in disguise" never reported in literature, and shows the presence of tangible risks for public health.

High-performance liquid chromatography-diode array and electrospray-mass spectrometry analysis of non-allowed substances in cosmetic products for preventing hair loss and other hormone-dependent skin diseases.

A simple high-performance liquid chromatography (HPLC) method with ultraviolet diode array (UV-DAD) and electrospray ionisation mass spectrometry (ESI-MS) detection has been developed for the determination of minoxidil, progesterone, estrone, spironolactone, canrenone, hydrocortisone and triamcinolone acetonide in cosmetic products. The presence of these substances in commercial cosmetic samples is prohibited. The compounds were separated by reversed phase chromatography with water (0.1% trifluoroacetic acid) and acetonitrile gradient elution and detected by UV-DAD at 230, 254 and 280 nm and by ESI-MS positive ionisation mode. Benzoic acid was used as internal standard. Linearity was studied with UV-DAD detection from 1.50 to 1,000 microg/ml or mug/g range, depending on the different compounds and type of cosmetic preparation and with ESI-MS in the 50-1,000 ng/ml or ng/g range. Good determination coefficients (r(2)>or=0.99) were found in both UV and ESI-MS. At three concentrations spanning the linear dynamic ranges of both UV-DAD and ESI-MS assay, mean recoveries were always higher than 90% for the different analytes. This method was successfully applied to the analysis of substances under investigations illegally added in cosmetic cream and lotions, sold on internet web sites to prevent hair loss and other hormone-dependent skin diseases, like acne and hirsutism.

HPLC determination of imidazole antimycotis in antidandruff cosmetic products.

A simple HPLC method for the determination of imidazole antimycotics in cosmetic antidandruff formulations has been developed. HPLC was carried out on a Discovery RP-Amide C16 column and spectrophotometric detection was performed at 220 nm. The initial mobile phase was a mixture of acetonitrile and aqueous 10(-3) M NaClO4 (pH 3.0) in the ratio of 15:85 (v/v); then a linear gradient up to 46% acetonitrile in 70 min, and up to 50% in 80 min. The extraction procedure has been validated by analyzing samples of shampoo and lotion spiked with 1% of the active principles. The recoveries were greater than 95% and the reproducibility was within 3%.

The reverse transcription inhibitor abacavir shows anticancer activity in prostate cancer cell lines.

BACKGROUND: Transposable Elements (TEs) comprise nearly 45% of the entire genome and are part of sophisticated regulatory network systems that control developmental processes in normal and pathological conditions. The retroviral/retrotransposon gene machinery consists mainly of Long Interspersed Nuclear Elements (LINEs-1) and Human Endogenous Retroviruses (HERVs) that code for their own endogenous reverse transcriptase (RT). Interestingly, RT is typically expressed at high levels in cancer cells. Recent studies report that RT inhibition by non-nucleoside reverse transcriptase inhibitors (NNRTIs) induces growth arrest and cell differentiation in vitro and antagonizes growth of human tumors in animal model. In the present study we analyze the anticancer activity of Abacavir (ABC), a nucleoside reverse transcription inhibitor (NRTI), on PC3 and LNCaP prostate cancer cell lines. PRINCIPAL FINDINGS: ABC significantly reduces cell growth, migration and invasion processes, considerably slows S phase progression, induces senescence and cell death in prostate cancer cells. Consistent with these observations, microarray analysis on PC3 cells shows that ABC induces specific and dose-dependent changes in gene expression, involving multiple cellular pathways. Notably, by quantitative Real-Time PCR we found that LINE-1 ORF1 and ORF2 mRNA levels were significantly up-regulated by ABC treatment. CONCLUSIONS: Our results demonstrate the potential of ABC as anticancer agent able to induce antiproliferative activity and trigger senescence in prostate cancer cells. Noteworthy, we show that ABC elicits up-regulation of LINE-1 expression, suggesting the involvement of these elements in the observed cellular modifications.

High performance liquid chromatography-diode array and electrospray-mass spectrometry analysis of vardenafil, sildenafil, tadalafil, testosterone and local anesthetics in cosmetic creams sold on the Internet web sites.

A simple high-performance liquid chromatography (HPLC) method with ultraviolet diode array (UV-DAD) and electrospray ionisation mass spectrometry (ESI-MS) detection has been developed for the determination of vardenafil, sildenafil, tadalafil, testosterone, procaine, lidocaine, prilocaine, and benzocaine in cosmetic creams sold as promising remedies for male erectile dysfunction and female genitals stimulation. The presence of these substances in commercial cosmetic samples is prohibited. Aliquots (1 g) of the cosmetic creams under investigation were diluted 1:100 in methanol, subjected to ultrasonic treatment, added with benzoic acid as internal standard, and analyzed by HPLC-DAD and HPLC-ESI-MS after a further 1:1000 dilution. The compounds were separated by reversed phase chromatography with water (0.02% trifluoroacetic acid) and acetonitrile gradient elution and detected by UV-DAD at 228, 255 and 290 nm and by ESI-MS positive ionisation mode. Benzoic acid was used as internal standard. Linearity was studied with UV-DAD detection from 2.5-7.8 to 250 microg/g range, depending on the different compounds and with ESI-MS in the 3.3-8.9 to 250 ng/g range. Good determination coefficients (r(2) > or = 0.99) were found in both UV-DAD and ESI-MS. Limits of quantifications ranged between 2.5 and 7.8 microg/g for HPLC-UV-DAD assay and between 3.3 and 8.9 ng/g for HPLC-ESI-MS assay depending on different analyzed substances. At three concentrations spanning the linear dynamic ranges of both UV-DAD and ESI-MS assay, mean recoveries were always higher than 90% for the different analytes and intra-assay and inter-assay precision always better than 15% and 12%. This method was successfully applied to the analysis of substances under investigations present in cosmetic creams, freely sold on the Internet web-sites.

Development of an HPLC method for the identification and dosage of non-allowed substances in cosmetic products. Part I: local anaesthetics and antihistaminics.

An HPLC method with ultraviolet detection coupled with a solid-phase extraction sample clean up was developed for the analysis of five local anaesthetics and four antihistaminics in cosmetic products. The presence of these compounds in commercial cosmetic samples is fordbidden. Extracts from real samples were applied to a solid-phase extraction C18 cartridge, and the analytes were eluted with 8:2 (v/v) acetonitrile/water containing 1% trifluoroacetic acid. HPLC separation was then performed for the identification and determination of the analytes using a Purospher RP-18 column, two gradient eluting systems and a photodiode-array detector. The accuracy of the method was verified by spiking experiments on home-made cosmetic samples. The analytical recoveries were satisfactory.