A Study on the Analysis of Isothiazolinone Components by High Performance Liquid Chromatography

고성능액체크로마토그래피에 의한 Isothiazolinone Components의 분석에 관한 연구

Introduction : Isothiazolinone product is one of new preservatives used in cooling tower, paper mill, and general industrial waters.l) It is also effective in controlling bacteria and fungi in the manufacture and storage of dispersed pigments, such as kaolin clays, titanium dioxide, calcium carbonate and others\ulcorner Its broad-spectrum activity, excellent physical and chemical compatibility with anionic, nonionic and cationic surfactants and most organic and inorganic compounds and low toxicity at recommended use levels provide formulators with an effective, economical, and environmentally acceptable alternative to other commercial biocides. It dose not contain or generate formaldehyde and is easy to formulate (1.5% solution is supplied as an aqueous solution), so that it gains advantage over the other preservatives. The active ingredients of the isothiazolinone product are unchlorinated compound (2-methyl-4-isothiazolin-3-one) and chlorinated one (5-chloro-2-methyl-4-isothiazolin-3-one). Methods preferred for the analysis of preservatives are chromatographic methods, especially high performance liquid chromatograph (HPLC). Although several methods were satisfactory in respect to separation, no offical method has been published for the isothiazolinone components. This study was performed to search for an alternative method in order to show flexible operating conditions of HPLC and to reduce assay time.

냉각탑, 제지산업, 일반 산업용수 등에 사용되는 산업용 방부제의 유효 성분 isothiazolinone components 즉, 2-methyl-4-isothiazolin-3-one(unchlorinated compound)과 5-chloro-2-methy14-isothiazolin-3-one(chlorinated compound)을 고성능액체크로마토그래피로서 분리, 정량하였다. 역상의 C$_{18}$ column (15 cmX3.9 mm I.D.)을 사용하였으며 자외선 검출기의 파장 254 nm에서 methanol-0.4% acetic acid(40 : 60)의 이동상, methanol-0.4% acetic acid(30: 70)의 추출 및 주입용매 조건으로 HPLC 분리를 시도한 결과 unchlorinated compound는 10~32,400 mg/l 범위에서, 그리고 chlorinated compound는 120~107,400 mg.l의 범위에서 직선성을 보였다. 내부 표준물질로서 dimethyl phthalate를 사용하였으며, unchlorinated compound, chlorinated compound 및 내부 표준물질의 순서로 븐리가 일어났고 총 분리시간은 6.41분이었다. 상기의 조건으로 시험물질을 분석, 정량한 결과 예측농도치에 근접한 수치를 얻었다.