串联质谱法（ESI—Q—MS／MS）快速测定布美他尼注射液的含量

目的建立一种简单、快速的布美他尼注射液主药含量测定方法。方法采用四极杆串联质谱法（tandem mass spectrometry，MS／MS）进行定性和定量测定．流动相：乙腈．水（80：20，v／v）．流速：150μL·min^-1，液-液法提取布美他尼，采甩与对照品质谱对照定性；选择性多反应监测操作模式（MRM）、内标法进行定量测定。结果串联质谱法检测布美他尼浓度在0．1-300μg·mL^-1范围内具有良好的线性关系（r=0．9981），最低检测极限LOD0．5ng·mL^-1．信噪比S／N=3．0。平均回收率为98．05％。用建立的方法同时测定了两个枇号的布美他尼注射液．检测结果分别为标示量的101．2％（批号20070901）和93．6％（批号20080201），符合药典90％．110％规定。结论用串联质谱法建立的布美他尼含量测定方法简单快速、灵敏度高、准确度好、专属性重复性好、稳定。可用于其注射液含量的质量控制。

Determination of bumetanide for injection by rapid tandem mass spectrometry

OBJECTIVE To establish a rapid and simple determination of principal agent for bumetanide injection. METHODS The qualitation and quantitation of bumetanide will be test with multiple reaction monitor （MRM）by tandem mass spectrometry（MS/MS）, mobile phase using the acetonitrile and water（80 ： 20, V/V）, bumetanide was extracted by ethyl acetate liquid-liquid and the quantitation was determinated with internal stan- dard. RESULTS There was a good correlation coefficient between 0.1-300μg· mL^-1 with tandem mass spec- trometry method, the correlation coefficient of linearity was 0.9981, the limit of detection of bumetanide was 0.5ng· mL^-1 and the signal-to-noise ratio was 3.0;the recoveries of the spiked samples were 98.05 %. Two different lots number bumetanide injection were detemianted at the same methods. The results showed that the test data by MS/MS were 101.2% （lot： 20070901） and 93.6% （lot： 20080201） according to the labeled con- tents.CONCLUSION The determination of bumetanide by tandem mass spectrometry was a simple and rapid method with high sensitivity and good specificity, and could be used for the quality control of bumetanide injection.