• 제목/요약/키워드: quality control of analytical result

검색결과 60건 처리시간 0.037초

생체시료 중 중금속 및 유기용제 대사물 분석의 실험실간 정도관리 프로그램 (Inter-laboratory Comparison for Analyses of Heavy Metals and Organic Solvent Metabolites in Biological Samples)

  • 양정선;이미영;박인정;강성규
    • 분석과학
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    • 제13권2호
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    • pp.258-267
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    • 2000
  • 1995년부터 실시해 온 산업보건 분야의 '유해물질 및 대사물 분석의 실험실간 정도관리 프로그램'(공식명: 특수건강진단기관 분석정도관리)의 5년간 실시 경과와 결과를 보고하고, 고찰을 통하여 우리나라 산업보건분야 실험실 서비스의 질관리를 위한 앞으로의 방향 등을 제시하고자 한다. 산업현장에서 많이 쓰이는 4가지 혈중 중금속과 5가지 유기용제 대사물에 대하여 연구원에서 제조된 표준시료를 분배하고 결과 분석값과 크로마토그람 등 관련 자료들을 분석하여 참가기관에 대한 분석능력 평가를 실시하였다. 연 2회 실시된 정도관리 결과는 인터넷 등을 통하여 고시하여 산업보건 관련 실험실들의 자율적인 질관리 서비스 경쟁을 유도하고, 관련 실험실 서비스의 사용자인 근로자, 사업주, 산업보건 관련자들의 알 권리를 충족시켜, 실험실의 분석데이타에 대한 객관적인 신뢰도를 확보하고 산업보건 서비스의 질 향상에 크게 기여하였다.

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국내 채소류와 과일류의 비타민 B6 함량 (Vitamin B6 Content of Vegetables and Fruits Cultivated in Korea)

  • 최소라;송영은;한현아;이송이;신소희;박진주
    • 한국식품영양학회지
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    • 제32권6호
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    • pp.745-752
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    • 2019
  • The purpose of this study was to determine the difference in vitamin B6 content according to the varieties, regions, and harvest times of vegetables and fruits in Korea using high performance liquid chromatography. We verified the accuracy of the analytical method with standard reference material 1849a and achieved reliability for internal analysis quality control with a mixture of cereal, whole wheat, and flour. As a result of the analysis, vitamin B6 contents (㎍/100 g) were 6.9~86.5 in peppers, 5.1~17.2 in paprika, 4.4~5.0 in strawberries, 4.0~52.9 in tomatoes, 7.7~7.8 in Chinese cabbage, 17.3~23.3 in radishes, 13.4~37.6 in apples, 2.3~12.7 in peaches, and 3.7~12.7 in grapes. In general, the difference in vitamin B6 content showed by varieties, harvest times, and regions. Peppers showed the most difference as 79.6 ㎍/100 g among the varieties, and apples showed a difference as 22.8 ㎍/100 g by regions. According to the harvest times in grape 'Mihwang', there was a difference of 7.5 ㎍/100 g. We will collect an amount of nutritional data on various food materials, and continue to build a reliable and integrated nutritional database. And then the database will be used in the 10th revision of the Korean Food Composition Table.

HPLC를 이용한 노루오줌 추출물의 Avicularin 및 Quercitrin 분석법 개발 (Analytical Method Development of Avicularin and Quercitrin in Astilbe chinensis Extract Using HPLC)

  • 권진관;정연우;서찬곤;홍성수;신현탁;정수영;최정준;김진규
    • 대한화장품학회지
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    • 제45권4호
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    • pp.333-340
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    • 2019
  • 본 연구는 노루오줌(Astilbe chinensis) 추출물을 기능성 화장품소재로 개발하기 위해 avicularin, quercitrin을 지표성분으로 선정하고, 품질관리를 위해 high performance liquid chromatography (HPLC)를 이용하여 분석법을 개발하였다. 분석용 칼럼은 Capcell Pak C18 MGII을, 이동상은 0.05% (v/v) trifluoroacetic acid (TFA)와 아세토니트릴을 사용하여 컬럼 온도는 30℃ 에서 유속 1.0 mL/min 로 검출파장은 254 nm에서 검출하였다. International conference on harmonization (ICH) 가이드라인(version 4, 2005)을 근거로 하여 특이성, 직선성, 정밀성, 정확성, 검출한계 및 정량한계를 분석하여 분석방법을 검증하였다. 분석결과, 검출한계 및 정량한계는 avicularin 0.094 및 0.285 mg/mL, quercitrin 0.031 및 0.095 mg/mL로 나타났으며, 검량곡선은 상관계수 값이 avicularin 0.99990, quercitrin 0.99994로 양호한 직선성을 보였고 정밀성 분석결과도 avicularin 0.59%, quercitrin 0.63% 이하로 확인되었다. 또한, 회수율은 avicularin 100.97 ~ 101.77%, quercitrin 100.18 ~ 100.32% 범위로 정확성이 있음을 알 수 있다. 따라서, 본 분석법은 노루오줌 추출물 지표성분의 분석법으로 적합한 시험법임이 검증되었다.

HPLC를 이용한 낙지다리 추출물의 (-)-­Epicatechin gallate 분석법 개발 (Analytical Method Development of (-)-Epicatechin gallate in Penthorum chinense Pursh Extract using HPLC)

  • 권진관;정연우;서찬곤;홍성수;최춘환;이지은;신현탁;정수영;김진규
    • 대한화장품학회지
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    • 제45권1호
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    • pp.87-93
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    • 2019
  • 본 연구는 낙지다리(Penthorum chinense Pursh) 추출물을 기능성 화장품소재로 개발하기 위해 (-)-epicatechin gallate를 지표성분으로 선정하고, 품질관리를 위해 High Performance Liquid Chromatography (HPLC)를 이용하여 분석법을 개발하였다. 분석에 사용된 칼럼은 Unison $US-C_{18}$ ($4.6{\times}250mm$, $5{\mu}m$, Imtakt, USA)을 사용하여 0.05% (v/v) trifluoroacetic acid (TFA)와 메탄올을 이동상 조건으로 컬럼 온도는 $30^{\circ}C$ 에서 유속은 1.0 mL/min 로 검출파장은 280 nm에서 검출하였다. International Conference on Harmonization (ICH) 가이드라인(version 4, 2005)을 근거로 하여 특이성, 직선성, 정밀성, 정확성, 검출한계 및 정량한계를 분석하여 분석방법을 검증하였다. 검출한계 및 정량한계는 각각 0.11 mg/mL 및 0.33 mg/mL로 나타났으며, 검량곡선은 상관계수값이 0.9999로 양호한 직선성을 보였고, 정밀성 분석결과도 0.6% 이하로 확인하였다. 또한, 회수율은 99.51 ~ 101.92% 범위로 정확성이 있음을 알 수 있다. 따라서, 본 분석법은 낙지다리 추출물의 지표성분의 분석법은 적합한 시험법임이 검증되었다.

HPLC 를 이용한 가는장구채 추출물의 Isoscoparin 분석법 개발 (Analytical Method Development of Isoscoparin in Silene seoulensis Extract Using HPLC)

  • 권진관;서찬곤;정연우;최용문;신현탁;정수영;최정준;김진규
    • 대한화장품학회지
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    • 제47권1호
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    • pp.57-63
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    • 2021
  • 본 연구는 가는장구채(Silene seoulensis) 추출물을 기능성 화장품소재로 개발하기 위해 isoscoparin을 지표성분으로 선정하고, 품질관리를 위해 high performance liquid chromatography (HPLC)를 이용하여 분석법을 개발하였다. 분석용 칼럼은 Unison US-C18을, 이동상은 0.05% (v/v) trifluoroacetic acid (TFA)와 메탄올을 사용하여 컬럼 온도는 35 ℃ 에서 유속 1.0 mL/min 로 검출파장은 330 nm에서 검출하였다. International conference on harmonization (ICH) 가이드라인(version 4, 2005)을 근거로 하여 특이성, 직선성, 정밀성, 정확성, 검출한계 및 정량한계를 분석하여 분석방법을 검증하였다. 분석결과, 검출한계 및 정량한계는 0.02 및 0.07 mg/mL로 나타났으며, 검량곡선은 상관계수 값이 0.99988로 양호한 직선성을 보였고 정밀성 분석결과도 0.46% 이하로 확인되었다. 또한, 회수율은 99.10 ~ 101.61% 범위로 정확성이 있음을 확인하였다. 따라서, 본 분석법은 가는장구채 추출물 지표성분의 분석법으로 적합한 시험법임이 검증되었다.

약물검사에서 관리시료의 농축을 이용한 보고 가능 범위의 설정에 대한 연구 (A Study of Reportable Range Setting through Concentrated Control Sample)

  • 장상우;김남용;최호성;박용원;윤근영
    • 대한임상검사과학회지
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    • 제36권1호
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    • pp.13-18
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    • 2004
  • This study was designed to establish working range for reoportable range in own laboratory in order to cover the upper and lower limits of the range in test method. We experimented ten times during 10 days for setting of reportable range with between run for method evaluation. It is generally assumed that the analytical method produces a linear response and that the test results between those upper and lower limits are then reportable. CLIA recommends that laboratories verify the reportable range of all moderate and high complexity tests. The Clinical Laboratory Improvement Amendments(CLIA) and Laboratory Accreditation Program of the Korean Society for Laboratory Medicine states reportable range is only required for "modified" moderately complex tests. Linearity requirements have been eliminated from the CLIA regulations and from others accreditation agencies, many inspectors continue to feel that linearity studies are a part of good lab practice and should be encouraged. It is important to assess the useful reportable range of a laboratory method, i.e., the lowest and highest test results that are reliable and can be reported. Manufacturers make claims for the reportable range of their methods by stating the upper and lower limits of the range. Instrument manufacturers state an operating range and a reportable range. The commercial linearity material can be used to verify this range, if it adequately covers the stated linear interval. CLIA requirements for quality control, must demonstrate that, prior to reporting patient test results, it can obtain the performance specifications for accuracy, precision, and reportable range of patient test results, comparable to those established by the manufacturer. If applicable, the laboratory must also verify the reportable range of patient test results. The reportable range of patient test results is the range of test result values over which the laboratory can establish or verify the accuracy of the instrument, kit or test system measurement response. We need to define the usable reportable range of the method so that the experiments can be properly planned and valid data can be collected. The reportable range is usually defined as the range where the analytical response of the method is linear with respect to the concentration of the analyte being measured. In conclusion, experimental results on reportable range using concentrated control sample and zero calibrators covering from highest to lowest range were salicylate $8.8{\mu}g/dL$, phenytoin $0.67{\mu}g/dL$, phenobarbital $1.53{\mu}g/dL$, primidone $0.16{\mu}g/dL$, theophylline $0.2{\mu}g/dL$, vancomycine $1.3{\mu}g/dL$, valproic acid $3.2{\mu}g/dL$, digitoxin 0.17ng/dL, carbamazepine $0.36{\mu}g/dL$ and acetaminophen $0.7{\mu}g/dL$ at minimum level and salicylate $969.9{\mu}g/dL$, phenytoin $38.1{\mu}g/dL$, phenobarbital $60.4{\mu}g/dL$, primidone $24.57{\mu}g/dL$, theophylline $39.2{\mu}g/dL$, vancomycine $83.65{\mu}g/dL$, valproic acid $147.96{\mu}g/dL$, digitoxin 5.04ng/dL, carbamazepine $19.76{\mu}g/dL$, acetaminophen $300.92{\mu}g/dL$ at maximum level.

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천연복합소재 LS-RUG-com의 기능성원료 표준화를 위한 산딸기 미숙과, 치자 및 유백피 지표성분의 분석법 검증 (Validation of Analytical Methods for Unriped Rubus crataegifolius, Gardenia jasminoides and Ulmus macrocarpa Marker Compounds for Standardization of Natural Complex LS-RUG-com Preparation as Functional Ingredient)

  • 이영익;표수진;이희진;윤혜정;손호용;조진숙
    • 생명과학회지
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    • 제34권1호
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    • pp.59-67
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    • 2024
  • 산딸기, 치자, 유백피의 혼합물인 복합 천연물 LS-RUG-com이 위염, 위궤양, 식도성 역류염 및 Helicobacter를 억제함을 확인한 바, LS-RUG-com을 건강기능식품 개별인정형 소재로 개발하고자 하였다. 본 연구에서는 소재 개발을 위한 LS-RUG-com 분석방법을 확립하고자 하였으며, 산딸기, 치자 및 유백피의 지표물질을 HPLC/UV system을 이용하여 분석방법을 최적화하였다. 본 연구에서는 분석법 validation을 입증하기 위하여 특이성(specificity), 정확성(accuracy), 정밀성(precision), 검출한계 및 정량한계(detection & quantitation limit) 및 직선성(linearity)을 평가하였으며, 그 결과 본 연구의 HPLC/UV 동시 분석법이 산딸기, 치자 분석에 적합하며, 신뢰성이 있음을 증명하였다. 또한 유백피의 HPLC/UV 단독 분석법이 적합하며 신뢰성이 있음을 증명하였다.

폴라로그래피를 이용한 $[^{201}Tl]$염화탈륨 주사액의 중금속 분석 (Analysis of Heavy Metals in $[^{201}Tl]$TICI Injection Using Polarography)

  • 전권수;서용섭;양승대;안순혁;김상욱;최강혁;이동훈;임상무;유국현
    • 대한핵의학회지
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    • 제34권4호
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    • pp.336-343
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    • 2000
  • 목적: $[^{201}Tl]$TICI주사액의 제조과정에서 안정동위원소인 $^{201}Tl$ 및 Cu, Pb의 중금속을 함유할 가능성이 있어 이러한 이물질을 확인하기 위한 방법으로 방사성 물질의 대기오염을 일으키지 않는 폴라로그래피의 분석 조건을 설정하고자 하였다. 대상 및 방법: 원자력병원에서 생산하고 있는 $[^{201}Tl]$-TlCl 주사액에 포함될 수 있는 중금속을 대상으로 하였다. 극미량의 중금속을 측정하기 위한 방법으로 BAS-50W 폴라로그래피를 이용하였고, 여기에 사용된 3 전극계는 작업전극인 DME, 기준전극인 Ag/AgCl 그리고 보조전극인 백금선을 이용하였다. 신속하고 재현성있는 분석을 위한 조건으로 기기의 분석 모드, 각 모드에 적합한 전극, 지지전해질, 석출시간 등의 치적 조건을 설정하였다. 결과: 폴라로그래피의 모드는 OSWSV 방법이 재현성과 감도면에서 가장 우수하였고, 작업전극은 DME와 Au 전극을 비교 실험한 결과 재현성 면에서 DME가 보다 좋은 결과를 보였다. 지지전해질은 염기성인 0.50 M KOH 용액, 산성인 1.0 M $HNO_3$, 용액, 중 성인 pH 7 phosphate 완충용액을 비교 실험하여 pH 7 phosphate 완충용액이 $Tl^+$$Cu^{2+}$를 분석하는데 가장 적합함을 확인하였다. 이를 바탕으로 중금속을 측정한 결과 $Tl^+$은 -450 mV, $Cu^{2+}$는 -50 mV에서 각각의 피크가 나타났고, 석출시간을 45초로 하였을 때 $Tl^+$의 경우 y=2.05E-$9{\chi}$+5.66E-9이고 $Cu^{2+}$의 경우는 y=1.23E-$8{\chi}$+1.23E-6의 선형 관계식을 얻었다. 결론: 이 방법에 의한 Tl과 Cu의 검출한계는 약 0.05 ppm이다. 이 방법을 현재 원자력병원에서 생산하고 있는 $[^{201}Tl]$TICl 주사액의 정도관리에 도입하여 중금속을 측정한 결과 약전에서 규정하고 있는 2 ppm 미만임을 확인하였고, 그 결과는 재현성, 정확도, 감도 및 간편성에서 모두 만족할 수 있었다. 이 방법은 $[^{201}Tl]$TlCl 주사액 뿐만 아니라 $^{67}Ga$ 주사액 및 기타 방사성의약품과 중금속 분석에도 응용할 수 있다.

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인구동태신고 및 통계조사의 개선방안 (A Study on Improvement of Vital Registration and Statistics System in Korea)

  • 신윤재
    • 한국인구학
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    • 제11권1호
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    • pp.58-75
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    • 1988
  • 1.Objectives of the Study It is a well known fact that a prompt and reliable data on demographic information is essential in a proper planning and evaluation of any program of national or community level. Especially vital statistics are an important demographic component among demographic information. Realizing the importance of vital statistics, the government has made some efforts for years to improve the vital registration system which has a close relationship with the production of vital statistics. However, it is still observed that there are some limitations in utilizing vital registration data due to considerable amount of vital events which are never registered and registered but not in time or inaccurately, even though vital registration system in Korea has sound legal basis. In this connection, the objectives of the study is as follows :(1) To examine some problems of the vital registration system in various aspects, (2) To make improvement programme of continuous Demographic Survey as a supplementary source of vital statistics, and (3) To find out some alternatives for making it possible to produce and utilize the reliable vital statistics by developing analytical methodologies on that. 2. Current Situation of Vital Registration System All the vital events, i.e. births, deaths, marriages and divorces, are to be registered in time under the Civil Registration Law, Statistics Law and Regulation on Vital Statstics as a duty of people. Some recent tendencies in each of recent registration are summarized as below: (1) The completeness of vital registration .Out of all births which are occurred during a year, around 75% of those compared to the estimates are registered in the year of occurrence. .In case of death registration, the percentage of registration in the year of occurrene has been gradually increased from 86.2% in the year of 1980, but it is still below the level of 90% compared to the estimates. .The percentage of registration for marriages and divorces in the year of occurrence out of total registered numbers was revealed to be 69% and 73% respectively in 1985. (2) Continuous Demographic Survey .It is a kind of sample survey for the purpose of producing reliable vital statistics which could not be provided by the vital registration. .It covers about 17, 000 sample households at national level and important information for vital events are collected in every month by 323 expertized enumerators who are regular staff of the government. .Although the result of the survey seems to be more reliable than of vital registration, the reliability of the data is still bellow the acceptable level if compared with relevant information from other sources such as population census or special surveys. 3. Problems of Vital Registration System There are four major obstacles in improving vital registration system in Korea; (1) In general, policy priority is not given on any programme of improving vital registration system. It is, therefore, very difficult to formulate comprehensive programme through having cooperation from related authorities and sufficient financial assistance. (2) In all the laws related and system itself, there is substantial degree of overlap and irrationality. Registration of each vital event is maintained according to several laws and regulation such as Civil Registration Law, Statistics Law, Resident Registration Law and Regulation on Vital Statistics. However they are mutually overlapped and overall supervision can not be done systematically due to lack of co-operation among the authorities concerned. (3) The administration of vital registration system seems to be working inefficiently, because of most of civil servants who are in charge of vital registration are lacking of conception on vital statistics and also there is a certain extent of regidity in handling the works. Therefore, they are doing their jobs in a passive way. (4) A substantial proportion of vital events occurred is not registered within the legal time limit (i.e. within one month after the occurrence in case of birth and death) or not registered forever. Some of social customs and superstitution seem to be the potential causes especially in case of births and deaths. 4. Recommendations for the Improvement of Vital Statistics (1) Reporting systems such as civil registration, vital statistics and resident registration should be integrated under the single law. Also, administrative supervision, personnel and budget with regard to the registration system should be under the control of a single ministry. (2) It is necessary to simplify the procedures and methods of reporting vital events, i.e., reducing number of sheets of the form, making corrections easily, reducing registration items, etc. (3) Continuous Demographic Survey as a supplementary source of vital registration should be improved and special ad-hoc surveys should be conducted wth regular interval. (4) In-depth analysis should be done using various sources of data on vital statistics. 5. Concluding Remarks From this study, we can notice that temporary campaign and motivation programs are not sufficient to improve the quality of vital statistics. Strong intentions and continuous efforts of the government are needed for the improvement of the vital registration system. Furthermore, most of the data collected through the registration are not properly analyzed and utilized, partly due to the lack of appreciation among high-level governmental officials of the need for vital statistics. It is, therefore, requested that long-term improvement programs of vital statistics be implemented with policy priority and continuous efforts be given to this purpose as a long-term goal of development in Korea.

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우리나라 농촌지역의 출산조절행태 및 출산조절행위의 결정요인 분석

  • 정경희;한성현;방숙
    • 한국인구학
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    • 제11권2호
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    • pp.33-53
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    • 1988
  • This study aimed at developing a desirable family planning policy and strategy by examining the current status of family planning practice in rural Korea and by indentifying the crucial factors which affect fertility control behavior. For this purpose, an analytical study was conducted, using the survey data collected in July 1985, on an interview basis, on 1, 440 married women living in the Soyi, Wonnam and Maingdong townships of Eumseong County(in North Chungcheong Province). This study population has the typical characteristics of rural areas, and the results of the analysis can be summarized as follows: 1. In regard to the demographic characteristics of the study population : their average age at marriage was 23.7, they had an average of 2.6 children( 1.3 boys, 1.3 girls) :10% experienced the death of their child (ren) :14% had spontaneous abortion(s) :4% weathered stillbirth(s) :35% went through induced abortion (s) : and 5.5% were currently pregnant. The average of their ideal numbers of children was 2.2, while 44% felt that they must have a son. 2. Looking at the contact rate with medical & health institutions, over the past 1 year, the visit rate to health subcenters was 43.7%, while 26.9% visited the (county) health center :59.6% had been to private clinics : and 41.5% went to the Soonchunhyang - Eumsung hospital : thus showing a relatively high rate of accessibility. 3. The utilization rate of family planning services was 76.5%, with tubectomy being the most prominent method at 52.3%, while the informants were health workers in 54.2% of the acceptors. Of the 8.4% who discontinued the use of contraceptive methods, only 26% did so due to want for pregnancy, natural infertility (meno - pause), or other reasons, while the remaining 74% stopped usage on account of side effects, failure in the methods themselves, and inconvenience of use, thus pointing to a situation where the proper choice of family planning methods have not yet been made. It can be noted that there is a strong motivation for early birth stopping as 35.3% practice family planning even with only one child, of which 38.3% have had sterilization operations. According to results of a multiple regression analysis, among the variables affecting contraception usage the most significant variable was the number of sons. 4. 34.8% experienced induced abortions. It was shown as a result of multiple regression analysis that the number of children and attitudes toward induced abortions extensively affected their frequency of abortions conducted. 5. In the regard to the relation between family planning and induced abortions, 33.7% of the women used both, while 52.0% of them used only the former(family planning), with only 1.4 % utilizing solely the latter(abortion), and 12.9% totally abstaining from fertility regulation : again, the discriminant analysis indicated that the choice of family planning and/or induced abortion was determined by the number of children and attitudes toward induced abortion. In view of the above mentioned results, the following are some comments and suggestions concerning problems related to the current family planning policies, in Korea : 1. It is difficult to expect a further quantitative expansion in family planning program operations, as there has been an excessive supply of target-oriented sterilization operations on women. From a maternal and child health care point of view, it will be desirable to have a diversification of service points in the future where family planning methods may be properly chosen, so that choices of methods which suit the mothers' characteristics and tastes may be made by the individuals themselves by strengthening their quality of family planning information services. 2. Along with the strengthening of the qualitative improvement of family planning services policies must be implemented to effectively promote the moral (ethical) deterrents to induced abortions and to preference for sons. From a maternal care standpoint, the social permissive norm toward induced abortion must be modified, and the bias towards son must be analyzed as the women with more daughters have a lower rate of family planning acceptance. Such changes in attitudes, however, can not be hoped to be accomplished with ad hoc policies, but will only be possible when an enhancement of the women's status(within the society) is brought about in a long - term perspective.

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