离子迁移谱法快速测定L-谷氨酰胺呱仑酸钠颗粒中有效成分含量

目的: 建立快速测定L-谷氨酰胺呱仑酸钠颗粒中有效成分含量的离子迁移谱方法. 方法 :采用离子迁移谱正模式测定L-谷氨酰胺含量,电离源电压3 kV;呱仑酸钠测定时为负模式,电离源电压2.6 kV;迁移管电压均为8 kV,电离源和迁移管温度均为180 ℃. 结果: L-谷氨酰胺和呱仑酸钠质量浓度均在10~200 μg · mL^-1范围内与峰面积线性关系良好,相关系数分别为0.998 2和0.997 4;定量限分别为10 μg · mL^-1和6 μg · mL^-1;L-谷氨酰和呱仑酸钠胺高、中、低3个浓度平均回收率均在97%~103%之间.每批样品连续测定6次,L-谷氨酰胺的平均含量分别为100.4%、101.0%和98.8%,RSD分别为2.2%、2.2%和2.3%;呱仑酸钠的平均含量分别为100.7%、101.7%和99.1%,RSD分别为2.7%、2.3%和2.7%. 结论: 离子迁移法适用于L-谷氨酰胺呱仑酸钠颗粒中有效成分含量测定.

Objective: To establish a rapid method for active pharmaceutical ingredients (APIs) detection in L-glutamine and sodium gualenate granules. Methods: A positive mode ion mobility spctrum (IMS) method was employed to detect the content of L-gutamine.The electrospray ionization (ESI) source voltage was 3.0 kV.Sodium gualenate was detected at the negative mode with source voltage at 2.6 kV.At the two modes,the drift tube voltages was both 8.0 kV.The ESI source and drift tube were both at the temperature of 180 ℃. Results: The linearity of L-glutamine and sodium gualenate was fine with the range of 10-200 μg · mL^-1 and the correlation coefficients were 0.998 2 and 0.999 7.And their LOQs were 10 μg · mL^-1 and 6 μg · mL^-1,respectively.The recoveries of L-glutamine and sodium gualenate in high,middle and low levels were all between 97%-103%.The samples of three batches were tested for six times continuously.The average contents of L-Glutamine were 100.4%,101.0% and 98.8%,and the RSDs were 2.2%,2.2% and 2.3%,respectively.And the average contents of sodium gualenate were 100.7%,101.7% and 99.1%,and the RSDs were 2.7%,2.3% and 2.7%,respectively. Conclusion: The established IMS method is suitable to detect the APIs of L-glutamine and sodium gualenate granules.

[1] SONG SG(宋树果),ZHOU M(周敏).Effect of Marzulene-s combined with ranitidine in treatin peptic ulcer(麦滋林-s加雷尼替丁治疗消化性溃疡)[J].New Drug Clin Remed(新药与临床),1997,16(3):77
[2] XU JX(许晋星).Determination of sodium gualenate in L-glutamine and sodium gualenate granules(麦滋林颗粒中呱仑酸钠含量测定方法的研究)[J].China Trop Med(中国热带医学),2009,5(9):885
[3] ZHANG ZH(张占辉),LIU QB(刘庆彬).Determination of sodium gualenate in compoud glutamine by RP-HPLC(反相高效液相色谱法测定复方谷氨酰胺中呱仑酸钠的含量)[J].Chin Hosp Pharm J(中国医院药学杂志),2003,23(3): 152
[4] SONG Y(宋一),PAN YQ(潘永泉).Determination of L-glutamine and sodium gualenate rapidly disintegrationg tablets by HPLC(HPLC法测定L-谷氨酰胺呱仑酸钠速崩片中L-谷氨酰胺组分的含量)[J].Chin Pharm Aff(中国药事),2007,21(5): 330
[5] WEN JC(文加才),LIU WF(刘文凤),YU L(俞仑).Determination of L-Glutamine(L-谷氨酰胺的含量测定方法)[J].Chin J New Drugs(中国新药杂志),2002,11(5):385
[6] SERGIO A,MANEL A,MARCELO B.A review of recent,unconventional applications of ion mobility spectrometry(IMS)[J].Anal Chim Acta,2011,703(5):114
[7] O'DONNELL RM,SUN XB,HARRINGTON PB.Pharaceutical applications of ion mobility spectrometry[J].Trends Anal Chem,2008,27(1): 44
[8] STRACHAN NJC,NICHOLSON FJ,OGDEN ID.An automated sampling system using ion mobility spectrometry for rapid detection of bacteria[J].Anal Chim Acta,1995,319(1/2): 63
[9] MIDEY AJ,PATEL A,MORAFF C,et al.Improved detection of drugs of abuse using high-performance ion mobility spectrometry with electrospray ionization (ESI-HPIMS)[J].Talanta,2013,116(15):77
[10] BRUINS AP.Mechanistic aspects of electrospray ionization[J].J Chromatogr A,1998,794(1/2): 245
[11] MANS DJ,CALLAHAN RJ,DUNN JD.Rapid-screening detection of acetildenafils,sildenafils and avanafil by ion mobility spectrometry[J].J Pharm Biomed Anal,2013,75(5): 153
[12] ZHANG F(张帆),LUO YC(罗域城).RP-HPLC simultaneous determiation of L-glutamine and sodium gualenate granules(反相高效液相色谱法同时测定L-谷氨酰胺呱仑酸钠颗粒中L-谷氨酰胺和呱仑酸钠的含量)[J].Chin J Pham Anal(药物分析杂志),2010,30(8): 1448