化工技术与开发
化工技術與開髮
화공기술여개발
TECHNOLOGY & DVELOPMENT OF CHEMICAL INDUSTRY
2014年
7期
45-47
,共3页
韦善怀%徐燕%韦志明%黄平%黄科润%穆允玲%莫友彬
韋善懷%徐燕%韋誌明%黃平%黃科潤%穆允玲%莫友彬
위선부%서연%위지명%황평%황과윤%목윤령%막우빈
气相色谱法%内标法%4-氯乙酰乙酸乙酯%手性4-氯-3-羟基丁酸乙酯
氣相色譜法%內標法%4-氯乙酰乙痠乙酯%手性4-氯-3-羥基丁痠乙酯
기상색보법%내표법%4-록을선을산을지%수성4-록-3-간기정산을지
gas chromatography%internal standard method%ethyl 4-chloroacetoacetate%chiral ethyl 4-chloro-3-hydroxybutyrate
采用气相色谱法测定4-氯乙酰乙酸乙酯不对称催化还原手性4-氯-3-羟基丁酸乙酯反应体系中相关组分的含量。选择手性色谱柱及1,3-丁二醇内标物为色谱条件，在此条件下各种物质能很好地分离，该方法的检出限为10.24~19.56 mg·L-1，相对标准偏差为0.42%~0.68%，加标回收率为97.7%~101.3%，其精密度和准确度均能满足常规分析要求。
採用氣相色譜法測定4-氯乙酰乙痠乙酯不對稱催化還原手性4-氯-3-羥基丁痠乙酯反應體繫中相關組分的含量。選擇手性色譜柱及1,3-丁二醇內標物為色譜條件，在此條件下各種物質能很好地分離，該方法的檢齣限為10.24~19.56 mg·L-1，相對標準偏差為0.42%~0.68%，加標迴收率為97.7%~101.3%，其精密度和準確度均能滿足常規分析要求。
채용기상색보법측정4-록을선을산을지불대칭최화환원수성4-록-3-간기정산을지반응체계중상관조분적함량。선택수성색보주급1,3-정이순내표물위색보조건，재차조건하각충물질능흔호지분리，해방법적검출한위10.24~19.56 mg·L-1，상대표준편차위0.42%~0.68%，가표회수솔위97.7%~101.3%，기정밀도화준학도균능만족상규분석요구。
A gas chromatographic method for the determination of pharmaceutical intermediates chiral ethyl 4-chloro-3-hydroxybu-tyrate from ethyl 4-chloroacetoacetate by the asymmetric hydrogenation was described. Chiral capillary column and 1,3-butanediol as internal standard were chosen as chromatographic conditions, in which all components could be separated and determined. The detection limit was less than 20mg/L, the RSD was 0.42%~0.68%and the recovery was 97.7%~101.3%.
