Objective: To explore the prepararation methods and rules of hair quality control samples which contained ketamine, norketamine or fluoroketamine, and the effects of different preparation and storage conditions on the performance of hair quality control samples. Methods: Different preparation conditions were compared, such as different types of soaking solutions, solutions with different target contents, different amount of blank hair etc. The performances of hair quality control samples which were prepared in different conditions were systematically analyzed, and eighteen kinds of hair quality control samples with different contents of targets and different forms were prepared according to the rules, ACN-DMSO (1∶1, v/v, added 0.02 mol·L-1 hydrochloric acid) was used to soak blank hair in different time periods to prepare hair quality control samples with a wide coverage. HPLC-MS/MS instruments and BEH C18(100 mm×2.1 mm, 1.7 μm) column were used to test the content of targets in hair. Column temperature was 40 ℃, the mobile phases were aqueous solution with 0.1%(v/v) formic acid (A)-acetonitrile aqueous solution with 0.1%(v/v) formic acid (B), gradient elution (0-9 min, 5%B→100%B; 9-11 min, 100%B; 11-11.1 min, 100%B→5%B; 11.1-13 min, 5%B, a flow rats of 0.4 mL·min-1, inject volume of 1 μL. The homogeneity, short term and long term stability in different storage conditions (temperature, humidity, light conditions, etc.) were also investigated. Results: The influences of different preparation conditions on the hair quality control samples were determined, soaking solutions had strong influences on the hair quality control samples, however the amount of blank hair had nearly no effects. All the samples prepared were uniform, F of each sample was lower than F0.05(table) (3.02) according to the F-test method, and all the samples were stable, during storage at room temperature, refrigerated or frozen conditions for 6 months, the contents of the target substances in each sample were monitored, all of RSDs were <12%, and the t values of each sample were < t(0.05)(table) (2.131 8) according to the T-test method. Conclusion: This study provides preparation rules of hair quality control samples and also provides detailed reference data for subsequent preparation and storage of related hair quality control samples.
WU Jian-mei, ZHANG Ting-ting, LI Jing, CHEN Jie
. Study on preparations of hair quality control samples containing ketamine, norketamine and fluoroketamine*[J]. Chinese Journal of Pharmaceutical Analysis, 2024
, 44(1)
: 158
-167
.
DOI: 10.16155/j.0254-1793.2024.01.16
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