[논문]Development of Analytical Method of Biotin in Complex Drugs and Dietary Supplements Using HPLC-UV

Huh, Yoon-Young; Kang, Yun-Pyo; Choi, Yong-Seok; Park, Jeong-Hill; Kwon, Sung-Won

doi:10.4333/kps.2011.41.1.025

Development of Analytical Method of Biotin in Complex Drugs and Dietary Supplements Using HPLC-UV 원문보기

Journal of pharmaceutical investigation, v.41 no.1, 2011년, pp.25 - 30

Huh, Yoon-Young (College of Pharmacy and Research Institute of Pharmaceutical Sciences, Seoul National University) , Kang, Yun-Pyo (College of Pharmacy and Research Institute of Pharmaceutical Sciences, Seoul National University) , Choi, Yong-Seok (College of Pharmacy and Research Institute of Pharmaceutical Sciences, Seoul National University) , Park, Jeong-Hill (College of Pharmacy and Research Institute of Pharmaceutical Sciences, Seoul National University) , Kwon, Sung-Won (College of Pharmacy and Research Institute of Pharmaceutical Sciences, Seoul National University)

Abstract ▼ AI-Helper

Recently, Korean Food and Drug Administration (KFDA) has focused on developing quality control guidelines for all commercial products in Korea to enforce regulations, improve the quality control, and protect consumers by developing prevalently used and efficient analytical tools to determine and quantify target compounds. Because the Korean Pharmacopeia (KP) presents microbiological assays for biotin, which is laborious and time-consuming, this study is focused on applying HPLC-UV to detect and quantify biotin in complex drugs and dietary supplements like multi-vitamin. Biotin in complex drugs was extracted from methanol and analyzed using mobile phase with 10 mM potassium phosphate (monobasic, pH=3.0) in distilled water and acetonitrile. Gradient condition was used to successfully detect and quantify biotin within 20 minutes. Validation result for linearity was significant that average $r^2$ was 0.999 (n=3) and its relative standard deviation (RSD) was 0.0578% which was less than 2%. Using this method, quantification of biotin in complex drugs was completed successfully and recovery tests were finished that recovery percentage greater than 95% with relative standard deviation less than 2%.

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문제 정의

The purpose of this study was to develop a new analytical method for biotin in order to utilize in administrative performance. Since many precedents have not fully satisfied the ultimate goal of their usage (Miwa et al.

제안 방법

37×10^-1%, respectively. Finally, accuracy/system suitability test was done to confirm the accuracy of the method and applied to commercial complex drugs. As a result, the recovery percentages were calculated greater than 95% with RSD less than 2%.
972%) imply better accuracy of our method. Finally, inter-day validation was performed by running three different concentrations per day for three consecutive days. Table IV illuminates the areas for different concentrations with RSDs.
583%, which was less than 2%. Further, intra-day validation was carried out by repeating one set of five different concentrations for three times and each RSD value was calculated to verify intra-day repeatability. As shown in the Table III, the average RSD value was 0.
In this study, a solid analytical method for biotin was developed and successfully completed while adhereing to the method validation protocol set by the HPLC-UV. Therefore, this method could potentially become a quality control guideline that could provide low economic cost and simple procedures for easier approach to be performed in common laboratories.
, 2002). It introduced three parts of the experiment: linearity, precision, and accuracy/system suitability and in order to prove the linearity, five different concentrations were required, usually 80, 90, 100, 110 and 120% of standard solution. In this study, 150 ppm was determined 100%.
Recovery test was examined to determine the accuracy of the developed method and the system suitability for the analysis of biotin in commercial products and three complex tablet drugs were used to evaluate recovery and reproducibility of the method. Each drug was diluted and extracted using methanol to make 150, 165 and 180 ppm and each sample (n=3) was membrane filtered to remove impurities.
As a part of the validation of the analytical method, its repro ducibility was examined, first. System validation was performed by injecting a biotin standard solution of 150 ppm six times consecutively and each area was compared to obtain standard deviation and RSD. As presented in Table II, the RSD for system validation was confirmed as 0.
, 2004). The importance of this study is to provide simple procedure to prepare samples to run experiment within 30 min. and therefore, build a bridge that connects scientific research and practical application of analytical chemistry for administrative usage.
78×10^-2%). Then, precision was examined followed by system validation, intra-day validation, and inter-day validation. System valida tion requires six trials and intra- and inter-day validation need three trials.

대상 데이터

Samples used for recovery tests were referred to as Drug A (500 µg/tablet), B (165 µg/tablet) and C (300 µg/tablet). All samples were multi-vitamins tablets and twenty of them were weighted and grounded. Twenty tablets for each drug were weighted and finely grounded.
Samples used for recovery tests were referred to as Drug A (500 µg/tablet), B (165 µg/tablet) and C (300 µg/tablet).

성능/효과

Finally, accuracy/system suitability test was done to confirm the accuracy of the method and applied to commercial complex drugs. As a result, the recovery percentages were calculated greater than 95% with RSD less than 2%.
Required relative standard deviation (RSD) in the protocol is less than 2% in the case of three trials and the RSD for linearity in this study satisfied the requirement (5.78×10-2%).
Results for system validation, intra-, and inter-day RSD values were 5.83×10-2%, 9.72×10-2%, and 4.37×10-1%, respectively.

참고문헌 (16)

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