The Korean Journal of Pesticide Science (농약과학회지)

The Korean Society of Pesticide Science (한국농약과학회)
권호 표지

Improvement of Analytical Method for Residue Pesticides in Herbal Medicines Using Macroporous Diatomaceous Earth Column

다공성 규조토 컬럼을 이용한 한약재 중 잔류농약 분석법 개선

  • Hwang, Jeong-In (School of Applied Biosciences, Kyungpook National University) ;
  • Jeon, Young-Hwan (School of Applied Biosciences, Kyungpook National University) ;
  • Kim, Hyo-Young (School of Applied Biosciences, Kyungpook National University) ;
  • Kim, Ji-Hwan (School of Applied Biosciences, Kyungpook National University) ;
  • Ahn, Ji-Woon (School of Applied Biosciences, Kyungpook National University) ;
  • Seok, Da-Rong (School of Applied Biosciences, Kyungpook National University) ;
  • Lee, Yoon-Jeong (Medicine Research, Korea Food and Drug Administration) ;
  • Park, Ju-Young (Medicine Research, Korea Food and Drug Administration) ;
  • Kim, Do-Hoon (Medicine Research, Korea Food and Drug Administration) ;
  • Kim, Jang-Eok (School of Applied Biosciences, Kyungpook National University)
  • 황정인 (경북대학교 응용생명과학부) ;
  • 전영환 (경북대학교 응용생명과학부) ;
  • 김효영 (경북대학교 응용생명과학부) ;
  • 김지환 (경북대학교 응용생명과학부) ;
  • 안지운 (경북대학교 응용생명과학부) ;
  • 석다롱 (경북대학교 응용생명과학부) ;
  • 이윤정 (식품의약품안전청 생약연구과) ;
  • 박주영 (식품의약품안전청 생약연구과) ;
  • 김도훈 (식품의약품안전청 생약연구과) ;
  • 김장억 (경북대학교 응용생명과학부)
  • Received : 2011.06.02
  • Accepted : 2011.06.15
  • Published : 2011.06.30
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Abstract

The official analytical method of residue pesticides in herbal medicines by KFDA cannot be applied to all of the pesticides and herbal medicines because of various active materials in herbal medicines and various physicochemical properties of pesticides. Moreover, liquid-liquid partition uses harmful solvents such as methylene chloride and is consuming a lot of time and effort. In order to improve the problems, we have studied for the availability of the analytical method applying the macroporous diatomaceous earth (MDE) column instead of liquid-liquid partition to simultaneously analyze five pesticides in two dried herbal medicines. The results showed that the recovery rates of acetamiprid and azoxystrobin in Astragalus root by GC/ECD ranged from 89.6 to 94.1%, from 86.8 to 94.4%, respectively, and those of bifenthrin, chlorfenapyr, chlorpyrifos in Cnidii Rhizoma by GC/MS ranged from 83.6 to 88.4%, from 77.4 to 83.8%, from 82.6 to 84.3%, respectively. Also, the coefficients of variation (CV) for triplication ranged from 0.5 to 1.7%. The results satisfied the criteria of residue pesticide analysis, setting 70~120% for the recovery rate and below 10% for the coefficient of variation. The improved methods are safer to residue pesticide analysts, faster and less laborious than the KFDA official method.

식품의약품안전청에서 고시한 한약재 중 잔류농약 분석법에 따라 천궁 중 bifenthrin, chlorfenapyr 및 chlorpyrifos와 황기 중 acetamiprid, azoxystrobin을 분석한 결과 크로마토그램 상에 많은 간섭물질이 나타나고 회수율이 낮은 문제점이 나타났다. 이를 개선하기 위한 방법으로 액-액 분배 과정 대신 macroporous diatomaceous earth(MDE) 컬럼을 적용하고 정제 시 용출용매 조건을 최적화함으로써 회수율은 황기에서 acetamiprid 89.6~94.1%, azoxystrobin 86.8~94.4%, 천궁에서 bifenthrin 83.6~88.4%, chlorfenapyr 77.4~83.8%, chlorpyrifos 82.6~84.3%, 변이계수(CV)는 전체시료에서 0.5~1.7%로 나타나 잔류농약 분석기준인 70~120% 의 회수율과 10% 이내의 변이계수를 만족하였다. 액-액 분배 과정을 대신하여 MDE 컬럼을 적용함으로써 발암가능 물질로 분류된 methylene chloride 사용을 배제할 수 있어 분석자의 안전성을 증대시킬 수 있었다. 또한 발생하는 폐액의 감소와 전처리 시 노동력 및 시간의 절감, 분석자간의 재현성 양호 등의 이점도 얻을 수 있었다.

Keywords

Acknowledgement

Supported by : 식품의약품안전청

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