The development and validation of HPLC methods for the detection of drug and detergent traces on laboratory glassware in a pharmaceutical laboratory / Pride Mmakeletso Mothobi

• Main Author: Mothobi, Pride Mmakeletso
• Language: en
• Published: North-West University 2013
• Online Access: http://hdl.handle.net/10394/8467

Pharmaceutical contract testing laboratories carry a responsibility to ensure that medicine made available for consumption by patients is of the approved quality for their intended health use. Glassware is an essential tool in testing of pharmaceutical products. Glassware used in most pharmaceutical contract testing laboratories is nondedicated hence proper glassware cleaning procedures are essential. Contract testing laboratories need to perform glassware cleaning validation studies to verify that glassware used in the testing of medicines is adequately cleaned from one product to the next and to ensure that the cleaning procedures themselves do not contribute any unwanted residues to the glassware. The aim of this study was to develop and validate HPLC methods for the detection of drug and detergent residues recovered from glassware in a pharmaceutical contract testing laboratory. The objectives of the study were to: i. Develop and validate an HPLC method to detect selected glassware cleaning detergents; ii. Investigate the efficacy of the current in-house glassware cleaning protocol (manual and automatic cleaning); iii. Investigate the efficacy of cleaning detergents on glassware exposed to drugs; iv. Develop an efficient glassware cleaning protocol; v. Validate a glassware cleaning protocol for a pharmaceutical laboratory. Cleaned laboratory volumetric flasks of varying sizes were randomly used as samples. Glassware washed with the automatic laboratory glass-washer and manually washed glassware was subjected to the rinsing and swabbing sampling procedures. A standard addition and recovery procedure was also employed to prove that the cleaning procedure works and that the glassware is indeed clean after being hand washed or automatically washed with the glassware washer. The HPLC method was validated on an LC Agilent® 1100 DAD series system using a IJBondapak C18 (300 mm x 3.9 mm, 10 IJm). Acetonitrile: buffer containing 0.02 M hexanesulfonic acid sodium salt with the pH adjusted to 3.0 with phosphoric acid in the ratio 25:75 was used as mobile phase with the flow rate set at 1.0ml/min. UV detection set at 220 nm and the injection volume at 25 IJI. The regression line plot obtained was linear over a concentration range from 5000 IJg/ml to 15 000 IJg/ml for Ekon D concentrate® and a concentration range from 9700 IJg/ml to 39 000 IJg/ml for LaboCiean FT concentrate®. The correlation coefficient of 0.993 was obtained for Ekon D concentrate® and 0.999 for LaboCiean FT concentrate®. The detection limit and quantitation limit were1568 IJg/ml and 5228 IJg/ml for Ekon D concentrate®, and 917 IJg/ml and 3059 IJg/ml for LaboCiean FT concentrate®. The relative standard deviation (%RSD) obtained for both detergents were below 7.0%. The mean recovery of the method was 99.5%. In the results obtained detergent traces were recovered from approximately 16% of the total sampled hand washed glassware and in 13% of the hand washed glassware, drug contaminants were also recovered. From the machine washed sampled glassware 10% was contaminated with drug residues and none of the sampled machine washed glassware flasks were contaminated with soap residues. The HPLC method developed for the detection of detergent and drug traces recovered from laboratory glassware was a success. The automated glassware cleaning procedure was more efficient in the cleaning of laboratory glassware when compared to the manual cleaning procedure. Observation shows that the current in-house glassware cleaning protocol is efficient; however, the SOP is not followed properly. The developed HPLC method was proved to meet all the performance expectations and acceptance criteria for cleaning validation purposes. The aim of this study to develop and validate the HPLC method for the detection of drug and detergent traces recovered from laboratory glassware for a pharmaceutical contract testing laboratory was met. === Thesis (MSc (Pharmaceutics))--North-West University, Potchefstroom Campus, 2012