超高效液相色谱串联质谱法测定不同厂家生产的多潘立酮片中多潘立酮的含量
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摘要
目的建立超高效液相色谱串联质谱法(UPLC-MS/MS)测定多潘立酮片中多潘立酮含量的方法 ,比较不同厂家生产的多潘立酮片中多潘立酮的含量。方法采用BEH C18色谱柱(2.1 mm×50 mm,1.7μm),流动相为甲醇:2 mmol/L乙酸铵水溶液(85∶15,V/V),进样量2μL,柱温30℃,流速0.2 m L/min。采用多重反应监测模型(MRM)方式进行正离子模式检测。结果多潘立酮在3.0 min内分离良好,在10.6～5300 ng/m L浓度范围内与峰面积呈良好的线性关系,线性回归方程为Y=85.362 X+30 067,r=0.9959;其检测限为1.06 ng/m L,定量限为10.6 ng/m L,加样回收率为99.2%,相对标准偏差(RSD)为1.7%。不同厂家生产的多潘立酮片中多潘立酮的含量分别为10.016、10.147、10.092、10.123、10.109、10.075 mg,均符合2015年版《中华人民共和国药典》(二部)的要求。结论该方法简便、快速,重复性好,灵敏度高,适用于多潘立酮片的快速定量分析。
Objective To establish a method for the determination of domperidone in Domperidone Tablets by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS), and to compare the contents of domperidone in Domperidone Tablets produced by different manufacturers. Methods BEH C18 column(2.1 mm × 50 mm,1.7 μm) was used. The mobile phase was methanol∶2 mmol/L ammonium acetate aqueous solution(85∶15, V/V). The injection volume was 2 m L, the column temperature was 30℃, and the flow rate was 0.2 m L/min. Multiple Reaction Monitoring Model(MRM) was used for positive ion pattern detection. Results Domperidone was well separated within 3 min and showed a good linear relationship with peak area in the concentration range of 10.6-5300 ng/m L. The linear regression equation was Y = 85.362 X+30 067. The limit of detection was 1.06 ng/m L, and the limit of quantitation was10.6 ng/m L. The average recoveries was 99.2% with the relative standard deviation(RSD) being 1.7%. The contents of domperidone in Domperidone Tablets produced by different manufacturers were 10.016, 10.147, 10.092, 10.123, 10.109 and 10.075 mg respectively, which met the requirements of the 2015 edition of the Pharmacopoeia of the People′s Republic of China(Part Ⅱ). Conclusion The method is simple, rapid, reproducible and sensitive. It is suitable for rapid quantitative analysis of domperidone.
Objective To establish a method for the determination of domperidone in Domperidone Tablets by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS), and to compare the contents of domperidone in Domperidone Tablets produced by different manufacturers. Methods BEH C18 column(2.1 mm × 50 mm,1.7 μm) was used. The mobile phase was methanol∶2 mmol/L ammonium acetate aqueous solution(85∶15, V/V). The injection volume was 2 m L, the column temperature was 30℃, and the flow rate was 0.2 m L/min. Multiple Reaction Monitoring Model(MRM) was used for positive ion pattern detection. Results Domperidone was well separated within 3 min and showed a good linear relationship with peak area in the concentration range of 10.6-5300 ng/m L. The linear regression equation was Y = 85.362 X+30 067. The limit of detection was 1.06 ng/m L, and the limit of quantitation was10.6 ng/m L. The average recoveries was 99.2% with the relative standard deviation(RSD) being 1.7%. The contents of domperidone in Domperidone Tablets produced by different manufacturers were 10.016, 10.147, 10.092, 10.123, 10.109 and 10.075 mg respectively, which met the requirements of the 2015 edition of the Pharmacopoeia of the People′s Republic of China(Part Ⅱ). Conclusion The method is simple, rapid, reproducible and sensitive. It is suitable for rapid quantitative analysis of domperidone.
引文
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[18]张宏伟,龚韬,严文利,等.高效液相色谱法测定不同厂家银翘解毒片中连翘酯苷A的含量[J].中国医药导报,2013,10(6):102-104.
[19]孙冬梅,林晓燕,李素梅,等.复方芪麻胶囊的质量标准研究[J].中国药房,2017,28(18):2553-2556.
[20]姚艺新,华芳,洪远林,等.川芎药材、饮片及其中成药抗血小板聚集活性的生物检定方法学研究[J].中草药,2017,48(11):2249-2254.
[21]赵军,徐媛,王庆伟,等.复方木香丸质量标准的提高[J].中国医药导报,2017,14(6):146-150.
[22]张肖建,朱梅羿,常云凤,等.不同厂家川芎配方颗粒的质量对比分析[J].中国医院用药评价与分析,2018,18(6):736-738,742.
[23]姚东,包永睿,王帅,等.芦黄参花胶囊质量标准研究[J].中国医药导报,2017,14(1):8-11.
[2]汪传臻,蔡朝敏.铝碳酸镁联合多潘立酮治疗胆汁反流性胃炎的效果观察[J].河南医学研究,2018(13):1.
[3]袁溢苒,童明霞,周丽峰,等.多潘立酮联合用药治疗胆汁反流性胃炎的疗效观察[J].中国处方药,2018,16(1):52-53.
[4]李艳华.多潘立酮联合复方消化酶治疗功能性消化不良的疗效观察[J].中国现代医生,2017,55(28):39-41.
[5]宋颖,陈敏纯,贾艳艳,等.多潘立酮口腔崩解片在健康人体的药动学和生物等效性[J].中国医院药学杂志,2012,32(10):775-779.
[6]庄晓庆.HPLC法测定多潘立酮片含量及含量均匀度[J]齐鲁药事,2007,26(5):278-280.
[7]庄瑞,李绍峰.HPLC法测定多潘立酮片的含量及含量均匀度[J].数理医药学杂志,2009,22(4):487-488.
[8]贺玉峰.HPLC法测定多潘立酮片的含量[J].中国药品标准,2006,7(4):40-42.
[9]易路遥,熊蔚.高效液相色谱法测定马来酸多潘立酮片的含量[J].实用中西医结合临床,2016,16(10):77-79.
[10]李鹏飞,王燕,童卫杭,等.液相色谱-串联质谱法测定人血浆中多潘立酮浓度[J].中国临床药理学杂志,2012,28(3):208-211.
[11]余鹏,阳国平,冉黎灵,等.LC-MS/MS法测定人血浆中多潘立酮的浓度[J].药物分析杂志,2011,31(4):619-624
[12]程小桂.基于代谢酶的威麦宁胶囊与多潘立酮相互作用研究[D].南京:南京中医药大学,2014.
[13]吴憩,姚鑫.UPLC-MS-MS测定不同厂家银杏叶提取物中4种萜内酯的含量[J].中国实验方剂学杂志,2016,22(15):60-63.
[14]吴婷,张军,居文政,等.HPLC-MS-MS法测定人血浆中多潘立酮浓度的不确定度分析[J].中国药事,2012,26(5):459-462.
[15]王秋石,李湘晖,纪宏宇.LC-MS/MS法测定人血浆中多潘立酮的浓度[J].中国药师,2012,15(2):224-226.
[16]罗亚男,许毓,李娜.HPLC-MS/MS检测人血浆中多潘立酮[J].光谱实验室,2011,28(6):2969-2972.
[17]谢君,吕玲燕,冯星月,等.UPLC-MS/MS法测定多潘立酮口腔崩解片的含量[J].实用药物与临床,2018,21(3):302-304.
[18]张宏伟,龚韬,严文利,等.高效液相色谱法测定不同厂家银翘解毒片中连翘酯苷A的含量[J].中国医药导报,2013,10(6):102-104.
[19]孙冬梅,林晓燕,李素梅,等.复方芪麻胶囊的质量标准研究[J].中国药房,2017,28(18):2553-2556.
[20]姚艺新,华芳,洪远林,等.川芎药材、饮片及其中成药抗血小板聚集活性的生物检定方法学研究[J].中草药,2017,48(11):2249-2254.
[21]赵军,徐媛,王庆伟,等.复方木香丸质量标准的提高[J].中国医药导报,2017,14(6):146-150.
[22]张肖建,朱梅羿,常云凤,等.不同厂家川芎配方颗粒的质量对比分析[J].中国医院用药评价与分析,2018,18(6):736-738,742.
[23]姚东,包永睿,王帅,等.芦黄参花胶囊质量标准研究[J].中国医药导报,2017,14(1):8-11.