Currently, ultraviolet-visible spectrophotometry and titration methods are used for assay tests of tramadol hydrochloride injection and raw material in the Korean Pharmacopoeia XI (KP XI). Titration has also been used in the British Pharmacopoeia (BP 2013) for the assay test of tramadol hydrochlorid...
Currently, ultraviolet-visible spectrophotometry and titration methods are used for assay tests of tramadol hydrochloride injection and raw material in the Korean Pharmacopoeia XI (KP XI). Titration has also been used in the British Pharmacopoeia (BP 2013) for the assay test of tramadol hydrochloride, and the HPLC assay for tramadol hydrochloride raw material has been used in the United States Pharmacopeia (USP 39). In this study, we developed an alternative HPLC assay method for tramadol hydrochloride injection that is up to date and specific, and employs the same method as tramadol hydrochloride capsules. Validation of the HPLC method was conducted to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of the calibration curves in the desired concentration range was good ($r^2$ > 0.9999). RSDs of intra-day precision obtained were 0.05-0.08 % and inter-day precision obtained were 0.08-0.19 %. Accuracy was obtained with recoveries in the range of 98.16 % and 100.90 %. As a result of the system's suitability, the RSD of both retention time and the peak area obtained were 0.07 %. The values of the plate number and tailing factor of tramadol hydrochloride obtained were 7076 and 1.16, respectively. Because of the intermediate precision and robustness of the developed assay, it is expected to become a valuable tool for revising the Korean Pharmacopoeia (KP XI).
Currently, ultraviolet-visible spectrophotometry and titration methods are used for assay tests of tramadol hydrochloride injection and raw material in the Korean Pharmacopoeia XI (KP XI). Titration has also been used in the British Pharmacopoeia (BP 2013) for the assay test of tramadol hydrochloride, and the HPLC assay for tramadol hydrochloride raw material has been used in the United States Pharmacopeia (USP 39). In this study, we developed an alternative HPLC assay method for tramadol hydrochloride injection that is up to date and specific, and employs the same method as tramadol hydrochloride capsules. Validation of the HPLC method was conducted to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of the calibration curves in the desired concentration range was good ($r^2$ > 0.9999). RSDs of intra-day precision obtained were 0.05-0.08 % and inter-day precision obtained were 0.08-0.19 %. Accuracy was obtained with recoveries in the range of 98.16 % and 100.90 %. As a result of the system's suitability, the RSD of both retention time and the peak area obtained were 0.07 %. The values of the plate number and tailing factor of tramadol hydrochloride obtained were 7076 and 1.16, respectively. Because of the intermediate precision and robustness of the developed assay, it is expected to become a valuable tool for revising the Korean Pharmacopoeia (KP XI).
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문제 정의
For the above reasons, the objective of the present work is to develop a reliable, simple, affordable HPLC method for quantitation of tramadol hydrochloride in injection. Validation was conducted following the International Conference on Harmonization (ICH) and Korean Food and Drug Administration (KFDA) Validation Protocols.
제안 방법
Calibration curves were prepared by taking appropriate volume of tramadol hydrochloride stock solution and diluting with water to obtain final concentrations of 20; 60; 100; 150; 200 and 250 µg/mL and used for evaluation of the linearity, accuracy, precision.
Experiments were conducted on Shimadzu HPLC system consisted of following components: DGU – 20A5R Degasser, two LC – 20 AD pumps, SIL – 20A autosampler, SPD-20A UV – Vis Detector, CBM – 20A communication bus module (Shimadzu Corporation, Kyoto, Japan) and CO-965 Column Oven (Jasco Corporation, Tokyo, Japan).
Method was validated accordingly to ICH Q2 (R1) guideline with regard to linearity, precision, accuracy and robustness.
Precision (relative standard deviation, RSD %) of the method were assessed by six analyses in a day (Intra – day) and in three different days (Inter – day) of standard solutions at concentrations corresponding to 80, 100, 120 % of analysis concentration (80; 100 and 120 µg/mL).
The precision of the method was assessed by determining the intra-day assay relative standard deviation (RSD %) of the analysis (n = 6) of standard solutions at three concentrations: 80; 100 and 120 µg/mL).
대상 데이터
Experiments were conducted on Shimadzu HPLC system consisted of following components: DGU – 20A5R Degasser, two LC – 20 AD pumps, SIL – 20A autosampler, SPD-20A UV – Vis Detector, CBM – 20A communication bus module (Shimadzu Corporation, Kyoto, Japan) and CO-965 Column Oven (Jasco Corporation, Tokyo, Japan). In intermediate precision validation, Agilent 1100 HPLC system included G1379A Degasser, G1312 Binary Pump, G1313 Auto-sampler, G1316 Colcom (Column Oven) and G1314AVWD Detector (Agilent Technology, Santa Clara, USA) was used.
Accuracy was expressed as recovery rates evaluated by standard addition method: three concentrations (80; 100 and 120 µg/mL) were spiked into 100 µg/mL sample solution. The experiments were performed in triplicate.
성능/효과
Results of recovery studies by standard addition method were ranged from 98.16 % to 100.90 % (Table 3). This also suggested that there was no interference from excipients in determining content of tramadol hydrochloride in injections.
참고문헌 (7)
Ministry of Food and Drug Safety, The Korean Pharmacopoeia, 11th Edition, Republic of Korea (2014)
National Cancer Institute, https://ncit.nci.nih.gov/ncitbrowser/ConceptReport.jsp?dictionaryNCI_Thesaurus&nsNCI_Thesaurus&code
The United States Pharmacopeial Convention, The United States Pharmacopeia, USP 39 NF 34, United States (2016).
Medicines & Healthcare Products Regulatory Agency, British Pharmacopoeia, 7th Edition, United Kingdom (2013).
ICH Guideline. Q2(R1): validation of Analytical Procedures: Text and Methodology Q2(R1) in ICH Harmonised Tripartite Guideline (2005).
Ministry of Food and Drug Safety No. 2009-173 (2009. 12. 15), Republic of Korea.
Ministry of Food and Drug Safety, No. C0-2012-2-005 (2012. 09. 19), Republic of Korea.
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