中国药师
中國藥師
중국약사
CHINA PHARMACIST
2014年
11期
1980-1983
,共4页
王茉莉%庞文哲%张菁%朱建平
王茉莉%龐文哲%張菁%硃建平
왕말리%방문철%장정%주건평
交沙霉素%交沙霉素片%高效液相色谱法%有关物质
交沙黴素%交沙黴素片%高效液相色譜法%有關物質
교사매소%교사매소편%고효액상색보법%유관물질
Josamycin%Josamycin tablets%HPLC%Related substance
目的：采用反相高效液相色谱法对交沙霉素原料及交沙霉素片中的有关物质进行分析。方法：采用Ultimate-AQ-C18色谱柱(250 mm ×4.6 mm,5μm),流动相A为0.2 mol·L-1四丁基硫酸氢铵-0.2 mol·L-1磷酸氢二钠(pH 3.0)-乙腈-水(3∶5∶24∶68),流动相B为0.2 mol·L-1磷酸氢二钠一水合物(pH 3.0)-乙腈-水(5∶50∶45),线性梯度洗脱。流速为1.5 ml·min-1,检测波长为232 nm,柱温为50℃。结果：交沙霉素主峰与杂质A、B、C、D、E相邻各峰间分离度均较好；交沙霉素主峰与其保留时间为1.1倍处杂质峰的分离度大于1.7。交沙霉素最低检出限为1.43 ng。交沙霉素原料和交沙霉素片中杂质A、B含量在1.5%以下,杂质D所占比例在2.0%以下,杂质E所占比例在3.0%以下,交沙霉素其它最大杂质所占比例在1.0%以下,总杂质所占比例在12%以下。交沙霉素原料中杂质C所占比例在1.0%以下,而交沙霉素片中杂质C所占比例在3.0%以下。结论：本方法灵敏度高,重现性好,专属性强,结果准确可靠,可以有效地分析交沙霉素原料及交沙霉素片中有关物质。
目的：採用反相高效液相色譜法對交沙黴素原料及交沙黴素片中的有關物質進行分析。方法：採用Ultimate-AQ-C18色譜柱(250 mm ×4.6 mm,5μm),流動相A為0.2 mol·L-1四丁基硫痠氫銨-0.2 mol·L-1燐痠氫二鈉(pH 3.0)-乙腈-水(3∶5∶24∶68),流動相B為0.2 mol·L-1燐痠氫二鈉一水閤物(pH 3.0)-乙腈-水(5∶50∶45),線性梯度洗脫。流速為1.5 ml·min-1,檢測波長為232 nm,柱溫為50℃。結果：交沙黴素主峰與雜質A、B、C、D、E相鄰各峰間分離度均較好；交沙黴素主峰與其保留時間為1.1倍處雜質峰的分離度大于1.7。交沙黴素最低檢齣限為1.43 ng。交沙黴素原料和交沙黴素片中雜質A、B含量在1.5%以下,雜質D所佔比例在2.0%以下,雜質E所佔比例在3.0%以下,交沙黴素其它最大雜質所佔比例在1.0%以下,總雜質所佔比例在12%以下。交沙黴素原料中雜質C所佔比例在1.0%以下,而交沙黴素片中雜質C所佔比例在3.0%以下。結論：本方法靈敏度高,重現性好,專屬性彊,結果準確可靠,可以有效地分析交沙黴素原料及交沙黴素片中有關物質。
목적：채용반상고효액상색보법대교사매소원료급교사매소편중적유관물질진행분석。방법：채용Ultimate-AQ-C18색보주(250 mm ×4.6 mm,5μm),류동상A위0.2 mol·L-1사정기류산경안-0.2 mol·L-1린산경이납(pH 3.0)-을정-수(3∶5∶24∶68),류동상B위0.2 mol·L-1린산경이납일수합물(pH 3.0)-을정-수(5∶50∶45),선성제도세탈。류속위1.5 ml·min-1,검측파장위232 nm,주온위50℃。결과：교사매소주봉여잡질A、B、C、D、E상린각봉간분리도균교호；교사매소주봉여기보류시간위1.1배처잡질봉적분리도대우1.7。교사매소최저검출한위1.43 ng。교사매소원료화교사매소편중잡질A、B함량재1.5%이하,잡질D소점비례재2.0%이하,잡질E소점비례재3.0%이하,교사매소기타최대잡질소점비례재1.0%이하,총잡질소점비례재12%이하。교사매소원료중잡질C소점비례재1.0%이하,이교사매소편중잡질C소점비례재3.0%이하。결론：본방법령민도고,중현성호,전속성강,결과준학가고,가이유효지분석교사매소원료급교사매소편중유관물질。
Objective: To establish a determination method for the related substances in josamycin and josamycin tablets by HPLC. Methods:High performance liquid chromatography was used. The column was Ultimate-AQ-C18(250 mm ×4.6 mm,5 μm), the mobile phase respectively was mobile phase A of 0. 2 mol·L-1 tetrabutylammonium hydrogen sulphate R-0. 2 mol·L-1 disodium hydrogen phosphate(pH 3. 0)-acetonitrile R-water(3∶5∶24∶68) and mobile phase B of 0. 2 mol·L-1 disodium hydrogen phosphate (pH 3. 0)-acetonitrile R-water(5∶50∶45). The flow rate was 1. 5 ml·min-1 with the detection wavelength of 232nm. The column temperature was 50℃. Results:The main component josamycin had a good separation with the other related substances. The resolution between josamycin and the related substances with the relative retention time of 1. 1-fold of josamycin was above 1. 7. The detection limit of josamycin was 1. 43ng. In josamycin raw materiel and josamycin tablets, the percentage of related substance A and B was less than 1. 5%. The percentage of related substance D was below 2. 0%. The percentage of related substance E was less than 3. 0%. The percentage of the other maximum related substances was less than 1. 0%. The percentage of all related substances was less than 12%. The percentage of related substance C was less than 1. 0% in josamycin raw materiel while 3. 0% in josamycin tablets. Conclusion:The method is accurate, sensitive and reliable in the determination of related substances in josamycin and josamycin tablets.
