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(1)
[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，1.7 μm)，流动相为甲醇：2 mmol/L乙酸铵水溶液(85∶15，V/V)，进样量2 μL，柱温30℃，流速0.2 mL/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/mL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/mL，定量限为10.6 ng/mL，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。
[关键词] 超高效液相色谱串联质谱法;不同厂家;多潘立酮;含量测定
[中图分类号] O657.63;TS207.5 [文献标识码] A [文章编号] 1673-7210(2019)03(a)-0033-04
[Abstract] 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 mL， the column temperature was 30℃， and the flow rate was 0.2 mL/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/mL. The linear regression equation was Y = 85.362 X+30 067. The limit of detection was 1.06 ng/mL， and the limit of quantitation was 10.6 ng/mL. 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.
[Key words] Ultra performance liquid chromatography-tandem mass spectrometry; Different manufacturers; Domperidone; Content determination
多潘立酮片是一種合成的苯丙咪唑类衍生物，为外周多巴胺受体阻滞剂，作用较强，主要作用于胃壁上的多巴胺受体而发挥胃动力效应，可增加食道下部括约肌张力，防止胃-食管反流，增强胃蠕动，促进胃排空，协调胃与十二指肠运动，抑制恶心、呕吐，并能有效地防止胆汁反流，不影响胃液分泌[1-4]。现大多采用高效液相色谱法测定多潘立酮片的含量[5-9]，而采用液相色谱串联质谱法(LC-MS/MS)测定其血药浓度的较多[10-12]。目前，国内共有多个厂家拥有多潘立酮片的生产批文，但其质量可能不完全一致。为保证临床用药、安全有效，本研究采用超高效液相色谱串联质谱法(UPLC-MS/MS)测定不同厂家生产的多潘立酮片中多潘立酮的含量。此法简便易行，准确度高，精密度灵敏度好，有利于更好地控制产品质量。, http://www.100md.com(耿晶 吕玲燕 冯星月)
[关键词] 超高效液相色谱串联质谱法;不同厂家;多潘立酮;含量测定
[中图分类号] O657.63;TS207.5 [文献标识码] A [文章编号] 1673-7210(2019)03(a)-0033-04
[Abstract] 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 mL， the column temperature was 30℃， and the flow rate was 0.2 mL/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/mL. The linear regression equation was Y = 85.362 X+30 067. The limit of detection was 1.06 ng/mL， and the limit of quantitation was 10.6 ng/mL. 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.
[Key words] Ultra performance liquid chromatography-tandem mass spectrometry; Different manufacturers; Domperidone; Content determination
多潘立酮片是一種合成的苯丙咪唑类衍生物，为外周多巴胺受体阻滞剂，作用较强，主要作用于胃壁上的多巴胺受体而发挥胃动力效应，可增加食道下部括约肌张力，防止胃-食管反流，增强胃蠕动，促进胃排空，协调胃与十二指肠运动，抑制恶心、呕吐，并能有效地防止胆汁反流，不影响胃液分泌[1-4]。现大多采用高效液相色谱法测定多潘立酮片的含量[5-9]，而采用液相色谱串联质谱法(LC-MS/MS)测定其血药浓度的较多[10-12]。目前，国内共有多个厂家拥有多潘立酮片的生产批文，但其质量可能不完全一致。为保证临床用药、安全有效，本研究采用超高效液相色谱串联质谱法(UPLC-MS/MS)测定不同厂家生产的多潘立酮片中多潘立酮的含量。此法简便易行，准确度高，精密度灵敏度好，有利于更好地控制产品质量。, http://www.100md.com(耿晶 吕玲燕 冯星月)