Study on the structure of an unknown impurity in carboplatin injection and the relationship with the excipient / 药学学报

The study was designed to establish a 2D UPLC-QTOF method to extrapolate the structure of an unknown substance in carboplatin injection and its relationship with the excipient. By using phenyl-hexyl column (250 mm×4.6 mm, 5 μm) with mobile phase consisting of tetrabutylammonium sulfate buffer (pH 7.5) and acetonitrile in gradient elution mode, an unknown impurity in carboplatin injection was found and quantitatively determined. Then a 2D UPLC-QTOF, HSS T3 column (100 mm×2.1 mm, 1.7 μm) was employed to confirm the molecular weight and the structure of the unknown impurity (electrospray ionization source, positive ion mode, MSE mode) with mobile phase consisting of 0.1% formic acid and acetonitrile. The relationship among impurities, API and excipient was investigated by accelerated stability test with ICP-MS/MS, ICP-AES. Results showed that disodium edetate in the formulation interacted with carboplatin producing an unknown impurity containing platin, and induced the increase of 1,1-cyclobutanedicarboxylic acid. The research should be done on the rationality of the addition of disodium edetate in such injections containing heavy metals.

Determination of disodium edetate in nalmefene hydrochloride injection by HPLC / 国际药学研究杂志

Objective To establish a high performance liquid chromatography (HPLC) method for the determination of disodium edentate (EDTA-2Na) in nalmefene hydrochloride injection. Methods Content of EDTA-2Na in nalmefene hydrochloride injection was determined by HPLC. C18 Column was used. The mobile phase consisted of 0.3% tetrabutylammonium hydroxide solution-wateracetonitrile (20: 45: 35) with a flow rate of 1.0 ml/min, and the detection wavelength was 254 nm. The column temperature was 30°C and the injection volume was 20 µl. Results The quantification limit and detection limit were 0.199 and 0.060 µg/ml, respectively; the linear equation for the disodium edetate was Y=10.125X-0.216, and the calibration curves were linear within the range of 2.4593~ 7.3780 µg/ml (r=1.000). Each concentration of the average recovery was between 98~102% (n=9) (RSD%=0.58%). Conclusion The method can be used for the determination of EDTA-2Na in nalmefene hydrochloride injection, which is convenient, fast, sensitive and reproducible, with good precision, specificity and accuracy.

Establishment of an anesthetic protocol for semen collection by electroejaculation in six-banded armadillos (Euphractus sexcinctus Linnaeus, 1758) / Estabelecimento de um protocolo anestésico para coleta de sêmen por eletroejaculação em tatus-peba (Euphractus sexcinctus Linnaeus, 1758)

The aim was to verify the effects of different anesthetic protocols used during electroejaculation (EEJ) in six-banded armadillos (Euphractus sexcinctus). Four sexually matured animals were physically restrained and subjected to semen collection by the EEJ following three treatments: The control group consisted of no use of anesthesia; in the others, the anesthetic combinations xylazine/ketamine/propofol or butorphanol/ ketamine/propofol were administered. For each group, twelve procedures were conducted for EEJ. Semen was evaluated for volume, color, aspect, motility, sperm concentration, morphology, viability, and functional membrane integrity. The highest efficiency (100% ejaculates) was achieved when the control group was used; the xylazine/ketamine/propofol association provided only 11 ejaculates from a total of 12 attempts (91.6% efficiency), while only 4 ejaculates (33% efficiency) were obtained with butorphanol/ketamine/propofol (P<0.05). Both protocols provided rapid induction and relaxation enough to perform the EEJ. In the use of butorphanol/ketamine/propofol, the animals recovered at 16.5±1.5min, a time shorter than in the use of xylazine/ketamine/propofol protocol, 20.7±1.0min (P>0.05). The semen volume and sperm concentration obtained in the use of xylazine/ketamine/propofol association were significantly higher than those verified for butorphanol/ketamine/propofol protocol. In conclusion, the xylazine/ketamine/propofol association is indicated for anesthesia of six-banded armadillos submitted to EEJ.(AU)

Objetivou-se verificar os efeitos de diferentes protocolos anestésicos usados durante a eletroejaculação (EEJ) em tatus-peba (Euphractus sexcinctus). Quatro animais sexualmente maduros foram contidos fisicamente e submetidos à coleta de sêmen por EEJ, seguindo três tratamentos: o grupo controle consistiu do não uso de anestesia; nos outros, foram administradas combinações anestésicas de xilazina/cetamina/propofol, ou butorfanol/cetamina/propofol. Para cada grupo, foram conduzidos 12 procedimentos de EEJ. O sêmen foi avaliado para volume, cor, aspecto, motilidade, concentração de espermatozoides, morfologia, viabilidade e integridade funcional da membrana. A mais alta eficiência (100% de ejaculados) foi alcançada quando o grupo controle foi utilizado; a associação de cetamina/xilazina/propofol forneceu apenas 11 ejaculados de um total de 12 tentativas (de eficiência 91,6%), enquanto apenas quatro ejaculados (eficiência de 33%) foram obtidos com butorfanol/cetamina/propofol (P<0,05). Ambos os protocolos forneceram rápida indução e relaxamento suficientes para executar a EEJ. Na utilização de butorfanol/cetamina/propofol, os animais se recuperaram em 16,5±1,5min, um tempo mais curto do que no uso de xilazina/cetamina/protocolo de propofol, 20,7±1,0min (P>0,05). O volume de sêmen e a concentração espermática obtidos no uso da associação xilazina/cetamina/propofol foram significativamente maiores do que os verificados para o protocolo butorfanol/cetamina/propofol. Em conclusão, a associação de cetamina/xilazina/propofol é indicada para anestesia de tatus-peba submetidos à EEJ.(AU)

Determinación tomográfica de la prevalencia de forma y tamaño de los rebordes residuales en pacientes edentados / Tomographic determination of residual ridges shape and size prevalence in edentate patients

INTRODUCCIÓN: el objetivo de esta investigación fue determinar tomográficamente la prevalencia de forma y tamaño de los rebordes residuales en pacientes edentados y su asociación con edad, sexo y reborde residual superior e inferior. MÉTODOS: se evaluaron 722 tomografías tomadas del centro de diagnóstico de UniCIEO, entre 2010 y 2012, de las cuales se obtuvieron 102 imágenes de rebordes residuales, 70 superiores y 32 inferiores, de 73 pacientes (46 mujeres, 27 hombres) con rangos de edad entre 24.67 y 90.17 años. La evaluación de forma y tamaño del reborde residual fue definido a través de nueve plantillas, generadas por el software Galaxis 3D, del sistema Cone beam GALILEOS (Sirona Dental Systems Inc., Bensheim, Germany). RESULTADOS: la prevalencia de forma y tamaño del reborde residual superior fue: ovoide grande 48.6%, triangular grande 42.9%, triangular mediano 4.3%, cuadrado grande 2.9%, ovoide mediano 1.4%; en inferior ovoide grande 93.8%, cuadrado grande 6.25%. CONCLUSIONES: la mayor prevalencia de forma y tamaño del reborde residual fue la ovoide grande, tanto en el maxilar superior como en el inferior. No se encontró asociación entre forma y tamaño con ninguna de las variables estudiadas.

INTRODUCTION: the objective of this tomographic study was to determine residual ridges shape and size prevalence in edentate patients and its association with age, sex, and upper and lower residual ridge. METHODS: we evaluated 722 scans taken at the UniCIEO diagnostic center between 2010 and 2012, obtaining 102 residual ridges images, 70 of the maxilla and 32 of the mandible, from 73 patients (46 women and 27 men) aged between 24.67 and 90.17 years. The evaluation of residual ridge size and shape was achieved through nine templates generated by the Galaxis 3D computer program, of the Cone beam GALILEOS system (Sirona Dental Systems Inc., Bensheim, Germany). RESULTS: the prevalent shape and size of upper residual ridge were: large ovoid 48.6%, large triangular 42.9%, medium triangular 4.3%, large square 2.9%, medium ovoid 1.4%; and in the mandible they were: large ovoid 93.8%, and large square 6.25%. CONCLUSIONS: the most prevalent residual ridge size and shape was large ovoid both in the upper and lower maxilla. We found no association between shape/size and any of the variables under study.