초록 ▼

○ 연구목표
○ 국제적 동등성을 갖춘 표준시료를 제조, 공급하여 국제적인 수준의 검사능력관리 기반 마련
○ 검사능력 평가방안 및 표준시료 제조 가이드라인을 마련하여 과학적이고 합리적인 검사능력관리 체계 구축
○ 2010년도 검사능력관리 표준시료(의약품(한약재), 화장품) 제작

○ 연구내용
의약품 등 검사기관 검사능력관리 4개 분야를 위한 표준시료를 다음과 같이 제조하여 배포하였다. 균질성은 병간 상대표준편차로 표기하였다.
- 한약재 중 잔류농약 분야: 전초류 한약재 중 chlorpyrifo

○ 연구목표
○ 국제적 동등성을 갖춘 표준시료를 제조, 공급하여 국제적인 수준의 검사능력관리 기반 마련
○ 검사능력 평가방안 및 표준시료 제조 가이드라인을 마련하여 과학적이고 합리적인 검사능력관리 체계 구축
○ 2010년도 검사능력관리 표준시료(의약품(한약재), 화장품) 제작

○ 연구내용
의약품 등 검사기관 검사능력관리 4개 분야를 위한 표준시료를 다음과 같이 제조하여 배포하였다. 균질성은 병간 상대표준편차로 표기하였다.
- 한약재 중 잔류농약 분야: 전초류 한약재 중 chlorpyrifos, α-Endosulfan
(균질성 0.7 %, 0.6 %)
- 한약재 중 중금속 분야 : 종자류 한약재 중 카드뮴 (균질성 1.4 %)
- 화장품 분야 : 베이비 파우더 중 납 (균질성 0.46 %)
- 의약품 분야 : 이부프로펜 제제의 함량 (균질성 0.7 %)
이와 같이 제조된 표준시료는 최상위 측정법에 의하여 기준값을 설정하였으며, 균질성, 안정성 및 불확도를 평가하여 표준시료로서 매우 적절함을 입증하였다.
이 표준시료에 대한 제조 방법 및 기준값 인증 방법을 상세히 기술함으로써 향후 표준시료 제조기관이 프로토콜로 사용할 수 있도록 하였다.

○ 연구성과(응용분야 및 활용범위포함)
식품의약품안전청 의약품 등 검사기관의 검사능력관리 4개 분야 표준시료를 인증표준물질 수준으로 제조하여 보급하였다. 시료 배포 내역은 다음과 같다.
- 한약재(잔류농약) : 15 g x 2 병 x 7 개 기관
- 한약재(중금속): 30 g x 1 병 x 7 개 기관
- 화장품(납): 20 g x 1 병 x 8 개 기관
- 의약품(이부프로펜): 3 g x 1 병 x 4 개 기관
각 표준시료의 기준값을 국가표준 수준으로 제공함으로써 절대평가의 잣대를 제공하였다. 이로써 검사능력관리의 신뢰성을 제고함으로써 위생검사기관의 측정 능력을 향상시키는 밑거름이 되었다. 한편 표준시료 제조 및 기준값 인증 방법을 상세히 제공함으로써 향후 표준시료 제조 기관의 프로토콜로 사용할 수 있도록 하였다.

Abstract ▼

The aim of this project was to prepare and evaluate 4 reference materials (pesticide residues and hazardous elements in oriental herbal medicines, cosmetics, active ingredient content in pharmaceutical products) and to provide their reference values as national standards. Those reference materials w

The aim of this project was to prepare and evaluate 4 reference materials (pesticide residues and hazardous elements in oriental herbal medicines, cosmetics, active ingredient content in pharmaceutical products) and to provide their reference values as national standards. Those reference materials were provided to KFDA for proficiency test of official laboratories. Target measurands for each item were as follows: pesticide residues (chlorpyrifos, α-endosulfan) in dried leafy herbal medicine, cadmium in dried seed herbal medicine, lead in baby powder, ibuprofen content in analgesic tablet. Homogeneity is the most important aspect for reference materials, and we provided reference materials with qualities equivalent to certified reference materials (CRMs) with satisfactory homogeneity. In addition, we have proven short-term stabilities of materials for organic analysis such as pesticide residues and ibuprofen. Therefore,we provided reference materials which have relatively higher qualities compared to materials supplied in other international proficiency testing programs.
Relative standard deviation between different bottles which represents the homogeneity of each reference material was adequate for proficiency testing purposes. Homogeneities of the provided reference materials were less than 1/3 of the relative standard deviation (actually obtained or expected by Horwitz equation) among participating laboratories in all of the cases.Also. standard uncertainties of reference values, which include uncertainties due to sample inhomogeneity, were less than 1/3 of the relative standard deviation among participating laboratories in most of the cases. When the standard uncertainty of a reference value slightly exceeds the criteria due to the inherent properties of the material, the uncertainty including the inhomogeneity was combined to the standard deviation (s) of the study for evaluating z-score.The reference materials prepared for this study were thought to be satisfactory in terms of homogeneities and uncertainties of reference values for testing proficiency of testing laboratories. It was possible to provide these homogeneous materials due to the capability of producing CRMs as the National Metrology Institute.
Reference values provided by KRISS were certified at the level of national standards via primary measurement methods which were proven to have international equivalencies among National Metrology Institutes. Testing laboratories that use these reference values as standards for evaluating and attempting to fit their results to these values will approach the internationally recognized standards. These attempts will be the basis of satisfying international requirement of conformity for testing laboratories.
The reference materials were securely packaged and distributed to the testing laboratories. Materials for the analysis of pesticide residues and ibuprofen were distributed in ice boxes filled with ice packs. During the material distribution, presentations were given to explain the production process, homogeneity of the materials, cautionary measures during sample handling and analysis, and this dispelled any doubts of the participants and enhance the reliability of the proficiency testing.
In addition, with detailed description of the production and certification process of the reference materials, this report can be used for protocols for future production of reference materials.
Among four reference materials provided to KFDA for proficiency test of official laboratories in 2009, long-term stabilities of two reference materials (ginseng for pesticide residue analysis, acetaminophen content in pharmaceutical product) were tested and confirmed.