earticle

영어

Cleansing & Hygiene products were previously managed as industrial products by the Ministry of Health and Welfare and the Ministry of Trade, Industry and Energy. Currently, it has been managed under the「Cleansing & Hygiene Products Control Act」 to ensure safety and quality since April, 2018. In this study, we improved the test method of phthalate plasticizers (DBP, dibutyl phthalate; BBP, butylbenzyl phthalate; and DEHP, diethylhexyl phthalate) of「Cleansing & Hygiene Products Codex」. This study improved methods such as correcting conditions of columns and analysis. Samples were taken from synthetic resin of disposable swabs and pulverized using freezer mill, followed by n-hexane soxhlet extraction. The GC-MS (Gas chromatography-mass spectrometry) analysis was performed on DB-5MS column. The oven temperature is settled as follows: 110oC ramped to 320oC. The acquisition is performed on full scan (m/z=50-500) and SIM (Selected ion monitoring) mode. Target ions of DBP, BBP, DEHP were 223, 206, 279 m/z and reference ions were (149, 205), (91, 149), (149, 167) m/z on GCMS, respectively. The method was validated by specificity, linearity, accuracy and precision according to ICH(International council for harmonisation of technical requirements for pharmaceuticals for human use) guideline. The LOD (Limit of detection) and LOQ (Limit of quantitation) indicated 0.07~0.30 mg/L and 0.22~0.91 mg/L, approximately, and the linearity showed R2 over 0.99 in the range of 1.0~20.0 mg/L. The intra and inter-day accuracy ranged 83.74~97.51% and precision was 101.65% with the RSD (Relative standard deviation) less than 2.88%. To evaluate the applicability of method, commercial products were monitored. The monitoring results met the「Cleansing & Hygiene Products Codex」, which has an allowance limit of three phthalates less than 0.1%.

한국어

위생용품은 보건복지부 및 산업통상자원부에서 공산품으로 관리 하였으나, ‘18년 4월부터「위생용품 관리법」 에 따라 식약처에서는「위생용품의 기준 및 규격」(식약처 고시 제2018-80호)으로 품목별 기준규격을 설정하여 관 리하고 있으며, 본 연구에서는 일회용 면봉에 대한 프탈레이트계 가소제 (DBP(dibutyl phthalate), BBP(buthylbenzyl phthalate), DEHP(diethylhexyl phthalate), 3종)의 컬럼규격 및 분석조건 변경 등 시험방법 개선연구를 수행하였다. 전 처리는 면봉 중 합성수지제에 해당하는 부분을 채취하여 냉동분쇄 후 n-헥산으로 속실렛 추출하였다. 컬럼은 DB-5MS, 분석장비는 GC-MS(Gas chromatography-mass spectrometry)를 이용하였다. 오븐온도는 110oC~320oC 승온조건으로 설 정하였다. 검출범위는 50-500 m/z에서 SIM(Selected ion monitoring) 모드로 수행하였다. DBP, BBP, DEHP 정량이온 은 223, 206, 279 m/z, 정성이온은 (149, 205), (91, 149), (149, 167) m/z이었고, 분석법 밸리데이션은 특이성, 직선성, 정 확성, 정밀성, 검출한계, 정량한계 등을 ‘의약품 등 시험방법 밸리데이션’ 및 ‘ICH(International council for harmonisation of technical requirements for pharmaceuticals for human use) 가이드라인’을 참고하여 수행하였다. 직 선성은 1~20 mg/L 범위에서 R2은 0.99 이상이었으며, LOD(Limit of detection), LOQ(Limit of quantitation)는 각 0.07~0.30 mg/L, 0.22~0.91 mg/L이었다. 정확성은 83.74~97.51%, 정밀성 RSD(Relative standard deviation)는 2.88% 이 하의 결과를 얻었다. 시중 유통품 대상으로 시험법 적용성 검토결과 프탈레이트 3종 모두 기준규격인 총합의 0.1%이하로 나타났다.