Articles

Syrotchuk O.A., Kobets A.O., Tananaiko O.Y. Improvement of characteristics of HPLC-UV methods for determining trace amounts of substances in rinses during cleaning validation

UDC 543.544.5.068.7;615.074
DOI

Syrotchuk O.A., Kobets A.O., Tananaiko O.Y.

Improvement of characteristics of HPLC-UV methods for determining trace amounts of substances in rinses during cleaning validation

Cleaning of process equipment and laboratory glassware plays a crucial role in ensuring the quality and safety of medicinal products in the pharmaceutical industry. In this study, we investigated the possibilities of reducing the limit of quantification for the HPLC-UV method to determine small amounts of substances in rinses from process equipment. It is shown that the use of water-ethanol mixtures in combination with the pentafluorophenyl (SiO 2 -PFP) stationary phase allows for better retention of the model substance - caffeine compared to octadecylsylil stationary phase. For example, when using a Discovery HS PFP (SiO2-PFP) column and a mobile phase containing 40% ethanol in water, the retention factor was 0,7, while under the same conditions using Discovery HS C18 (SiO2-PFP), it was 0,2. The advantages of using of the ethanol over acetonitrile are also demonstrated, as when 40% acetonitrile was used in the mobile phase, a lower retention factor of 0,4 was obtained. The impact of the increasing of the injection volume on the characteristics of the chromatographic peak was also examined. It was shown that under certain conditions, the injection volume can be increased to 250 μl, resulting in lower limits of quantification. The study confirms the achievement of a low limit of quantification equal to 0,27 ng/ml when using the HPLC-UV method, making it effective for analyzing rinses during the validation of cleaning processes.
Keywords: HPLC, ethanol, caffeine, cleaning validation.

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