논문 상세보기
pp.237-245
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.
재료 및 방법
1. 시약 및 기구
2. 약용작물 시료
3. HPLC-UVD/MS 기기분석 조건
4. 표준검량선 및 분석정량한계 (limit of quantitation, LOQ)
5. 시료의 추출 및 분배
6. Florisil 흡착 크로마토그래피
7. 대표 약용작물에 대한 cyanazine의 회수율 시험
결과 및 고찰
1. HPLC 분석조건의 확립
2. 약용작물 시료의 cyanazine 추출 및 분배과정의 확립
3. Florisil 흡착 크로마토그래피 정제조건의 최적화
4. 약용작물 시료 중 cyanazine의 분석정량한계 및 회수율
5. LC/MS를 이용한 잔류분의 재확인
REFERENCES
