본 연구는 불법적으로 식품에 사용될 수 있는 부정물질 11종에 대한 안전관리 강화를 위해 정량 및 정성 분석이 가능한 HPLC-DAD와 LC-MS/MS를 검증하기 위해 수행 되었다. 확립된 시험법은 AOAC 가이드라인에 따라 직선성, 정밀성, 정량한계 및 회수율 등을 통해 유효성을 확인 하였다. 본 실험에서 정량한계를 포함하여 검량선을 작성 하였고, 모두 0.99 이상의 직선성을 확인하였다. 또한 정확성은 LC (90.0-106%), LC-MS/MS (83.0-114%) 이고, 정 밀도는10% 이하로 재현성이 우수하였다. 확립된 시험법은 식품 중 부정물질 안전관리 및 모니터링에 활용될 것으로 사료된다.

In this work, we developed an analytical method for determining 11 illicit compounds in dietary supplements using high-performance liquid chromatography and liquid chromatography-tandem mass spectrometry. Eleven target compounds, including those meant for weight loss (7-keto-dihydroepiandrosterone, buformin, metformin, phenformin, salbutamol, and tolbutamide), sexual enhancement (dihydroepiandrosterone), and relaxation (asarone, kavain, magnoflorine, and picamilon) were screened and confirmed in dietary supplements. Method validation was performed by evaluating the selectivity, linearity, limit of quantification (LOQ), accuracy, and precision according to the Association of Official Analytical Chemists guidelines. The linearity was > 0.993 for all analytes. The LOQs were ranged in 2.1-9.9 μg/mL (HPLC-DAD) and 0.002-0.008 μg/mL (LC-MS/MS). The accuracies (expressed as recovery) were 90.0-106% (HPLC-DAD) and 83.0-114% (LC-MS/MS). The precision (expressed as the relative standard deviation) was below 10% using HPLC and LC-MS/MS. The proposed method can be used for the surveillance of illicit compounds in dietary supplements.

ABSTRACT
Materials and Methods
    Reagents and chemicals
    Preparation of stock and standard solutions
    Sample Preparation
    LC-DAD analysis
    LC-MS/MS analysis
    Method validation
Results and Discussion
    Optimization of HPLC conditions
    Optimization of LC-MS/MS parameters
    Method validation
    Comparison of instrumental analysis
국문요약
References

• Dasom Shin(New Hazardous Substances Team, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
• Hui-Seung Kang(New Hazardous Substances Team, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) Correspondence to
• Hyung-soo Kim(New Hazardous Substances Team, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
• Guiim Moon(New Hazardous Substances Team, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)