中国药师
中國藥師
중국약사
CHINA PHARMACIST
2015年
6期
890-893
,共4页
熊婧%何积芬%吴建敏%宁保明
熊婧%何積芬%吳建敏%寧保明
웅청%하적분%오건민%저보명
格列喹酮片%含量测定%含量均匀度%高效液相色谱%液相色谱-质谱联用
格列喹酮片%含量測定%含量均勻度%高效液相色譜%液相色譜-質譜聯用
격렬규동편%함량측정%함량균균도%고효액상색보%액상색보-질보련용
Gliquidone tablets%Content determination%Content uniformity%HPLC%UPLC-MS
目的：：建立HPLC方法准确测定格列喹酮片的含量,解决现行质量标准中含量测定方法不专属、供试品溶液配制方法不合理的问题。方法：采用UPLC-MS联用技术对降解杂质进行分析,正负离子同时扫描和子离子扫描模式,色谱柱为AC-QUITY UPLC BEH C18柱(50 mm ×2.1 mm,1.7μm),流动相为水(用甲酸调节pH至3.5)(A)-乙腈(B)梯度洗脱。采用建立的HPLC法对格列喹酮片的含量进行测定,Agilent Zorbax SB-C18色谱柱(150 mm ×4.6 mm,5μm),流动相为水(用甲酸调节pH至3.5)-乙腈(37.5∶62.5),检测波长为230 nm,柱温30℃,流速为1.0 ml·min-1,进样体积为20μl。结果：格列喹酮在60.200~140.400μg·ml-1范围内与峰面积线性关系良好(r=0.9995),平均回收率为98.60%,RSD为0.6%(n=9)。结论：本方法结果准确可靠,专属性强,重复性好,可用于格列喹酮片含量及含量均匀度的测定。
目的：：建立HPLC方法準確測定格列喹酮片的含量,解決現行質量標準中含量測定方法不專屬、供試品溶液配製方法不閤理的問題。方法：採用UPLC-MS聯用技術對降解雜質進行分析,正負離子同時掃描和子離子掃描模式,色譜柱為AC-QUITY UPLC BEH C18柱(50 mm ×2.1 mm,1.7μm),流動相為水(用甲痠調節pH至3.5)(A)-乙腈(B)梯度洗脫。採用建立的HPLC法對格列喹酮片的含量進行測定,Agilent Zorbax SB-C18色譜柱(150 mm ×4.6 mm,5μm),流動相為水(用甲痠調節pH至3.5)-乙腈(37.5∶62.5),檢測波長為230 nm,柱溫30℃,流速為1.0 ml·min-1,進樣體積為20μl。結果：格列喹酮在60.200~140.400μg·ml-1範圍內與峰麵積線性關繫良好(r=0.9995),平均迴收率為98.60%,RSD為0.6%(n=9)。結論：本方法結果準確可靠,專屬性彊,重複性好,可用于格列喹酮片含量及含量均勻度的測定。
목적：：건립HPLC방법준학측정격렬규동편적함량,해결현행질량표준중함량측정방법불전속、공시품용액배제방법불합리적문제。방법：채용UPLC-MS련용기술대강해잡질진행분석,정부리자동시소묘화자리자소묘모식,색보주위AC-QUITY UPLC BEH C18주(50 mm ×2.1 mm,1.7μm),류동상위수(용갑산조절pH지3.5)(A)-을정(B)제도세탈。채용건립적HPLC법대격렬규동편적함량진행측정,Agilent Zorbax SB-C18색보주(150 mm ×4.6 mm,5μm),류동상위수(용갑산조절pH지3.5)-을정(37.5∶62.5),검측파장위230 nm,주온30℃,류속위1.0 ml·min-1,진양체적위20μl。결과：격렬규동재60.200~140.400μg·ml-1범위내여봉면적선성관계량호(r=0.9995),평균회수솔위98.60%,RSD위0.6%(n=9)。결론：본방법결과준학가고,전속성강,중복성호,가용우격렬규동편함량급함량균균도적측정。
Objective:To establish an HPLC method for the content determination of gliquidone tablets to improve the specificity of the content determination and the rationality of the preparation of test solution. Methods: A UPLC-MS system was used to analyze the degradation products with positive and negative ion scanning and sub-ion scanning. An ACQUITY UPLC BEH C18 column(2. 1 mm × 50 mm,1. 7 μm) was employed with the mobile phase consisting of water (adjustting pH to 3. 5 with formic acid)-acetonitrile with gradient elution. The HPLC method was performed on an Agilent Zorbax SB-C18 column(150 mm × 4. 6 mm,5 μm). Water (adjusing pH to 3. 5 with formic acid)-acetonitrile(37. 5∶62. 5) was used as the mobile phase. The detection wavelength was set at 230 nm. The column temperature was set at 30℃. The flow rate was 1. 0 ml·min-1 with the injection volume of 20μl. Results:A good linear re-lationship was obtained within the range of 60. 200-140. 400μg·ml-1(r=0. 999 5), and the average recovery was 98. 60% with RSD of 0. 6% (n=9). Conclusion:The method is accurate, reliable, specific and reproducible, which can be used in the determination of content and content uniformity of gliquidone tablets.
