高效液相色谱-二极管阵列检测器法测定苯磺顺阿曲库铵的有关物质  

Determination of Related Substances in Cisatracurium Besilate by HPLC- DAD

作　　者：杜云[1] 王磊 顾维[3] 

机构地区：[1]南京大学化学化工学院,江苏南京210093 [2]南京美嘉宁逸医药研究开发有限公司,江苏南京210093 [3]江苏省南京市妇幼保健院,江苏南京210004

出　　处：《中国药业》2015年第8期64-67,共4页China Pharmaceuticals

摘　　要：目的建立测定苯磺顺阿曲库铵中有关物质的高效液相色谱法。方法采用高效液相色谱-二极管阵列检测器法。流动相梯度洗脱,流动相A为1.02%磷酸二氢钾缓冲溶液（用磷酸调节p H至3.1）-甲醇-乙腈（75∶5∶20）,流动相B为1.02%磷酸二氢钾缓冲溶液（用磷酸调节p H至3.1）-甲醇-乙腈（50∶30∶20）;色谱柱为Thermo Syncronis C18柱（250 mm×4.6 mm,5μm）,流量为1.0 m L/min,柱温为30℃,进样体积为20μL,检测波长为280 nm。结果苯磺顺阿曲库铵质量浓度线性范围为0.005~1.0 g/L（r=0.999 9）,检测限为5 ng/m L（S/N≥3）;杂质E、杂质G、中间体Ⅻ和中间体ⅩⅢ的质量浓度线性范围分别为0.8~40.0μg/m L,1.2~60.0μg/m L,40~200μg/m L,1.6~80.0μg/m L（r≥0.999 8）,检测限分别为40 ng/m L,30 ng/m L,100 ng/m L,80 ng/m L（S/N≥3）。结论该法检测苯磺顺阿曲库铵的有关物质,灵敏度高、专属性强,结果准确可靠。Objective To establish a HPLC method for the determination of related substances in cisatracurium besilate. Methods HPLC-diode array detector（DAD） was adopted. The mobile phase was performed the gradient elution. The mobile phase A was 1.02% potassium dihydrogen phosphate buffer solution （adjusting to pH 3.1 with phosphoric acid）-methanol-acetontrile （75：5：20） and the mobile phase B was 1.02% potassium dihydrogen phosphate buffer solution（adjusting to pH 3. 1 with phosphoric acid）-methanol- acetontrile （50：30：20）. The separation of analyte was performed on a Thermo Syncronis Cls column（250 mmx4.6 mm,5μm）. The flow rate was 1.0 mL/min,the column temperature was set at 30 ℃ and the injection volume was 20μL. DAD was set at 280 nm. Results The linear range of cisatracurium besilate was 0. 005- 1.0 g/L（r =0. 999 9）,the minimum detection limit was 5 ng/mL（S/ N≥3）;the linear ranges of mass concentrations for impurity E and G,midbody Ⅻ andⅫ were 0. 8-40. 0 μg/mL, 1.2-60.0 μg/mL, 40 - 200 μg/mL and 1.6 - 80. 0 μg/mL（ r≥ 0. 999 8）, and the minimum detection limits were 40,30,100,80 ng/mL（ S/ N≥3 ）. Conclusion This method for determining the related substances in cisatracurium besilate is strongly specific, highly sensitive, accurate and reliable in the detection results.

关 键 词：高效液相色谱法 苯磺顺阿曲库铵 有关物质 阿曲库铵 

分 类 号：R927.2[医药卫生—药学] R971.2