ABSTRACT
The aim of this study was to validate a method for determining nine types of steviol glycoside and its derivatives in food and beverage products, using ultrahigh-performance liquid chromatography tandem mass spectrometry with electrospray ionization (UHPLC ESI MS/MS). The performance characteristics of the analysis method were determined along with their suitability for the intended use. Coefficient of determination (R2) calibration curves from 0.2 to 1.0 mg L-1 were in the ranges of 0.9911-0.9990, 0.9939-1.0000 and 0.9973-0.9999 for a beverage, yogurt and snack, respectively. Intra-day precisions in terms of percent relative standard deviation (% RSD) of concentration, at 0.2, 0.5 and 1.0 mg L-1, for the beverage, yogurt and snack were lower than 15% (1.1-9.3%). At all concentrations, percentage recoveries were in the accepted range of 70-120%. For the matrix effect study, matrix-matched calibration was used for all compounds, obtaining a linear concentration range from 0.2 mg L-1 to 1.0 mg L-1. Almost all matrix-matched results presented as percentage recoveries were within the accepted range of 80-120%. The limit of detection (LOD) for steviol glycosides ranged from 0.003 to 0.078 µg g-1, while the limit of quantitation (LOQ) ranged from 0.011 to 0.261 µg g-1. These results indicate that the modified test method can be applied to determine the presence of steviol glycoside and its derivatives in a wide range of sample matrices.
ABSTRACT
For proper handling of a product knowledge regarding its water content is essential. To provide fast, inexpensive and reliable results, the direct evaporation method of water in oil bath (EDABO) has been proven to be a viable alternative, at all stages of production of the Brazil nut. Therefore, adaptation and validation of the EDABO method for the almonds was developed using ten lots, five for each stage, maintaining the water content range between 3.73 and 29.13% w.b, which is the typical water content range for the product from the collection phase until its final marketing. The oil bath temperatures tested were 150° C to 200° C, from 10 to 10° C for the adaptation step. The results thus obtained were compared with the water content recorded for the same batch employing the vacuum oven method as the standard. In the adaptation step the most suitable temperature range was set. Next, the method was validated to test for the precision, accuracy and linearity of the pre-set temperature range. During this step, temperature of 150° C were observed to ensured water content results consistent with those determined by the standard method. In the validation step the temperature of 150° C revealed precision, accuracy and linearity and were comparable to the standard method. Therefore, considering the technical aspects for implementation of this method, it was concluded that 150° C temperature was validated.
Para o manuseio adequado de um produto, conhecimento do seu teor de água é essencial. Por fornecer resultados rápidos, baratos e confiáveis, o método de evaporação direta da água no banho de óleo (EDABO) é comprovadamente uma alternativa viável para se conhecer o teor de água do produto, em todas as fases de produção da castanha-do-brasil. Para isso o método EDABO para as amêndoas foi desenvolvido utilizando-se dez lotes, cinco para a fase de adaptação e os outros cinco para a fase de validação, mantendo a faixa de teor de água entre 3,73 e 29,13% b.u.. Esta é a faixa de teor de água típica para o produto a partir da fase de extração até sua comercialização final. As temperaturas do banho de óleo testadas foram 150 a 200 °C, a cada 10 °C durante a adaptação. Os resultados obtidos foram comparados com o teor de água registrado para o mesmo lote empregando o método da estufa a vácuo como o referência. Na etapa de adaptação foi definida a faixa de temperatura mais adequada. Em seguida, o método foi validado para testar a precisão, exatidão e linearidade da faixa de temperatura pré-definida. Durante a adaptação, somente a temperatura de 150 °C apresentou resultados de teor de água consistentes com aqueles determinados pelo método de referência. Na etapa de validação, a temperatura de 150 °C revelou precisão, exatidão e linearidade e foram equivalentes àqueles determinados pelo método da estufa a vácuo. Portanto, considerando os aspectos técnicos para a implementação deste método, concluiu-se que 150 °C de temperatura foi validado.
Subject(s)
Seeds , Water , Bertholletia , HumidityABSTRACT
OBJECTIVE: To provide a method for the microbial limit test of Anshenning oral liquid and carry out validation of the mothed. METHODS: The validation on the microbial limit test method was conducted in accordance with the counting method of bacteria, mycetes and yeasts and the control bacteria test method stated in the Appendix of China Pharmacopoeia(2010 edition). Culture dilution method was used in bacterium count and total combined molds and yeasts count; while routine method was used in the control bacteria test. RESULTS: The recoveries of test organisms in the control group 3 preparations by routine method were more than 70%. The recoveries of the test group were more than 70%. In the 3 control bacteria tests the negative control bacterias, was not found in the negative control group, while the control bacteria was found in the test group. CONCLUSION: The established method substances can eliminate the antimicrobial in Anshenning oral liquid is accurate, and comprehensive, and can be used for the microbial limit test of Anshenning oral liquid.
ABSTRACT
OBJECTIVE: To study the antimicrobial effect of 11 kinds of oral Chinese patent medicines and to establish microbial limit test method for them. METHODS: Common method and culture medium dilution method and sticked filter membrane method were used to do the recovery test in order to validate the scientificity and feasibility of established method. RESULTS: Danqi piantan capsule showed strong inhibition effect on Staphylococcus aureus and Bacillus subtilis. Xinshuning tablet, Fuzheng mixture, Shenkangning mixture, Qingshen xiaodu oral liquid had antimicrobial effect on Staphylococcus aureus to some extent. Banlangen granule had antimicrobial effect on Bacillus subtilis. The effect can be eliminated by culture medium dilution method. CONCLUSION: The common method can be used for the microbial limit test of Jiaoou capsule, Zhike ningsou capsule, Rongdanshi granule, Sanjie mingmu capsule, Jiangzhi ruanmai tablet. Dilution method can be used for the microbial limit test of Xinshuning tablet, Fuzheng mixture, Shenkangning mixture, Qingshen xiaodu oral liquid, Banlangen granule, Danqi piantan capsule. The common method is suitable for all kinds of specified microorganisms.
ABSTRACT
OBJECTIVE:To establish a method for the microbial limit test of 29 hospital preparations.METHODS:A validation on the microbial limit test method was conducted in accordance with the counting method of bacteria,mycetes and yeasts and the control bacteria test method stated in the Appendix of China Pharmacopoeia(2005 edition).RESULTS:The recoveries of test organisms in 16 of the total 29 preparations by routine method were less than 70%,and the test organisms were failed to be detected in 6 preparations in the control bacteria test.For test organisms to meet the standard in recovery rate,medium dilution method,membrane-filter procedure,centrifugal method,neutralization method or the combination of these methods were needed.CONCLUSION:The test sample should undergo validation on the microbial limit test method to ensure the correctness of test result.
