In this study, the effect of difference in gas phase media (between nitrogen and air) used for standard gas preparation was evaluated with respect to relative recovery of carbonyl compounds (CC). To this end, calibration analysis was carried out using gaseous CC standards (with the two media) containing five different CCs (acetaldehyde (AA), propionaldehyde (PA), butyraldehyde (BA), isovaleraldehyde (IA), and valeraldehyde (VA)). Derivatization of CCs was made, and the carbonyl hydrazones eluted via acetonitrile were analyzed by reverse phase HPLC for UV detection. As a result, the CC standards in N2 medium showed about 10% higher recovery than that of air medium. However, the difference in their relative recovery is in most cases not statistically significant. Consequently, it is concluded that the difference in gaseous media like N2 or air is unlikely to affect derivatization efficiency of CCs.

An effective method, use of a 2,4-dinitrophenylhydrazine (DNPH) derivatization and high-performance liquid chromatography (HPLC) with ultraviolet (UV) detection, has been used for separation carbonyl compounds. In particular, acetonitrile/water composition as a mobile phase could not separated acrolein/acetone and 2-butanone/ butyraldehyde. In this study, however, that"s compounds separated using acetonitrile/water/tetrahydrofuran as a mobile phase. The resolution was 1.48 and 1.46, respectively. Also, aldehydes and ketones was shown different decrease rate and increase resolution at increase tetrahydrofuran ratio. But butyraldehyde become coeluted methacrolein. Therefore, it is need to consider of mobile phase for separation of butyraldehyde.

In this study, the QA/QC test for the combined application of DNPH cartridge – HPLC/UV method was investigated in the collection and analysis of formaldehyde in air using three types of DNPH cartridge samplers made by three independent manufacturers. For these experiments, gaseous standards of formaldehyde (FA) were prepared at 7 concentration levels that fell in the range of 44.1~3400 nmol/mol. According to our analysis, the levels of cartridge blank (0.13 ~ 0.26 ng) are found to be fairly high to require routine check up for each experiment. The recovery patterns of FA were highly comparable between different cartridge products, when standard gases are supplied in the concentration range up to 177 nmol/mol. All 3 types of DNPH cartridge exhibited highly similar recovery rates at concentrations below 1.7 ㎛ol/mol, while the maximum recovery was attained from the product B. The overall results of our study suggest that one should calibrate the samples in the optimal range of recovery with routine check up of blank values.

대한민국 식품의약품안전처(식약처)는 포름알데하이드 분석법으로 2,4-dinitrophenylhydrazine (DNPH) 유도체화-고성능액체크로마토그래프법(HPLC)을 고시하고 있다. 본 연구는 고시법의 복잡한 시료 전처리 과정을 개선하여 화장품 분석에 편리하게 사용할 수 있는 유도체화법을 개발하고자 수행되었다. 전처리 법을 간단하게 하기 위하여 pH, 시간 및 온도 등 반응조건을 최적화하였다. 이 전처리법은 초산염 완충액(pH 5.0)을 사용한 검액의 pH 조정, 디클로로메탄을 사용한 액-액 분획 그리고 감압농축기를 사용한 증발건조와 같이 식약처 고시법의 복잡한 과정이 필요 없다. 유도체화 과정을 통하여 생성된 formaldehyde dinitrophenylhydrazone (formaldehyde-DNP)는 식약처의 시험방법을 약간 변형한 역상 HPLC법으로 분리하고 정량하였다. 2 ∼ 40 ppm 농도 범위의 표준액들을 가지고 수행한 검량선 작성 결과, 본 시험법은 상관계수 값 이 0.9999로 좋은 직선성을 보여주었다. 본 실험의 최소검출한계(LOD)와 최소정량한계(LOQ)는 각각 0.2 ppm과 0.5 ppm이었다. 또한 회수율 실험결과는 실험방법이 매우 정확하고 재현성이 높음을 보여주었다. 따라 서 본 연구에서 제안된 시험법은 화장품 중 포름알데하이드를 신속하게 분석하는데 적용될 수 있을 것이다.