본 연구는 HPLC-DAD/MS를 이용하여 농산물 중 triazine 계 제초제인 cyanazine의 잔류 분석법을 확립하였다. 대표 농산물은 사과, 배추, 고추, 현미 및 콩을 선정하였고, 아세톤을 첨가하여 추출된 cyanazine 성분을 dichloromethane 액-액 분배법과 florisil 흡착크로마토그래피법으로 정제하여 HPLCDAD/ MS 분석대상의 시료로 사용하였다. Cyanazine의 정량적 분석을 위한 최적 HPLC-DAD/MS 분석조건을 확립하였으며, 정량한계(LOQ)는 0.02 mg/kg 이었다. 각 대표 농산물에 대해 정량한계, 정량한계의 10배 및 50배 수준에서 회수율을 검토한 결과, 모든 처리농도에서 83.6~93.3% 수준을 나타내었으며, 반복 간 변이계수(CV)는 최대 2.8%를 나타내어 잔류분석 기준인 회수율 70~120% 및 분석오차 10% 이내를 충족시키는 만족한 결과를 도출하였고, 또한 LC/MS SIM을 이용하여 실제 농산물 시료에 적용하여 재확인 하였다. 이상의 결과로 신규 cyanazine의 HPLC-DAD/MS 분석법은 검출한계, 회수율 및 분석오차 면에서 국제적 분석기준을 만족하는 신뢰성이 확보된 정량 분석법으로 사용 가능할 것이다.

Background: Cyanazine is used as a pre-emergent herbicide once during the growing season to control weeds of many upland crops worldwide. This study aimed to establish a method to determined cyanazine residue levels in major medicinal crops by using high performance liquid chromatography-UV detection/mass spectometry (HPLC-UVD/MS). Methods and Results: Cyanazine residue was extracted with acetone from the raw products of four representative medicinal plants - Scutellaria baicalensis, Paeonia lactiflora, Platycodon grandiflorum and Angelica gigas. The extract was diluted with a large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. It was then purifined using optimized Florisil column chromatography. HPLC analysis conducted using an octadecylsilyl column allowed the successful separation of cyanazine from co-extractives of the samples, and the amount was sensitively quantified by ultraviolet absorption at 225 ㎚ with no interference. The accuracy and precision of the proposed method were validated by conducting recovery experiments on each medicinal crop sample fortified with cyanazine at two concentration levels per crop in triplicate. Conclusions: The mean recoveries ranged from 91.2% to 105.3% for the four representative medicinal crops. The coefficients of variation were less than 10%, irrespective of the sample types and fortification levels. The limit of quantification of cyanazine was 0.02 ㎎/㎏ as verified by the recovery experiment. A confirmatory method was performed by liquid chromatography/MS using selected-ion monitoring technique to clearly identify the suspected residue.