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자료유형
학술저널
저자정보
Nam Sook Kim (Ministry of Food and Drug Safety) Geum Joo Yoo (Ministry of Food and Drug Safety) Kyu Yeon Kim (Ministry of Food and Drug Safety) Ji Hyun Lee (Ministry of Food and Drug Safety) Sung-Kwan Park (Ministry of Food and Drug Safety) Sun Young Baek (Ministry of Food and Drug Safety) Hoil Kang (Ministry of Food and Drug Safety)
저널정보
한국분석과학회 분석과학 분석과학 제32권 제2호
발행연도
2019.4
수록면
35 - 47 (13page)

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In this study, high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was employed to detect 26 antidiabetic compounds in adulterated dietary supplements using a simple, selective method. The work presented herein may help prevent incidents related to food adulteration and restrict the illegal food market. The best separation was obtained on a Shiseido Capcell Pak® C18 MGII (2.0 mm × 100 mm, 3 μm), which improved the peak shape and MS detection sensitivity of the target compounds. A gradient elution system composed of 0.1 % (v/v) formic acid in distilled water and methanol at a flow rate of 0.3 mL/min for 18 min was utilized. A triple quadrupole mass spectrometer with an electrospray ionization source operated in the positive or negative mode was employed as the detector. The developed method was validated as follows: specificity was confirmed in the multiple reaction monitoring mode using the precursor and product ion pairs. For solid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL, and for liquid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL. Satisfactory linearity was obtained from calibration curves, with R² > 0.99. Both intra and inter-day precision were less than 13.19 %. Accuracies ranged from 80.69 to 118.81 % (intra/inter-day), with a stability of less than 14.88 %. Mean recovery was found to be 80.6-119.0 % and less than 13.4 % RSD. Using the validated method, glibenclamide and pioglitazone were simultaneously determined in one capsule at concentrations of 1.52 and 0.53 mg (per capsule), respectively.

목차

Abstract
1. Introduction
2. Materials and Methods
3. Method Validation
4. Method Application
5. Results and Discussion
6. Conclusions
References

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