目的:建立高效液相离子对色谱-串联质谱法.测定磺丁基醚-β-环糊精(SBE-β-CD)中杂质4-羟基丁磺酸钠和二磺烷基化醚钠.方法:采用Inertsil ODS-SP C18(4.6 mm× 250 mm,5μm)色谱柱;流动相为甲醇-10 mmol·L-1正戊胺溶液(30∶70),流速1.0 mL· min-1.离子源:电喷雾离子(ESI)源;负离子多反应监测模式测定,4-羟基丁磺酸钠和二磺烷基化醚钠的监测离子对分别为m/z 153.0/79.8和m/z 289.0/152.9.结果:4-羟基丁磺酸钠和二磺烷基化醚钠分别在0.1～5.0 ng· mL-1和0.4～20.0 ng· mL-1范围内线性关系良好(r＞0.999 6),定量限分别为0.01、0.04 ng· mL-1,平均加样回收率分别为96.2％、95.4％,RSD分别为3.8％、4.1％.3批供试品中4-羟基丁磺酸钠的含量依次为0.001 6％、0.001 3％、0.000 57％,二磺烷基化醚钠均低于检测限.结论:该方法专属性强、灵敏度高,可用于4-羟基丁磺酸钠和二磺烷基化醚钠的测定,为SBE-β-CD的质量控制提供了便捷方法,同时也为其他烷基磺酸钠盐化合物的分析提供了参考.

目的建立GC法测定磺丁基醚-β-环糊精（betadex sulfobutyl ether sodium,SBE-β-CD）中杂质1,4-丁烷磺内酯。方法采用分散液液微萃取处理样品。50μL氯仿作为萃取剂,0.5 mL乙腈作为分散剂,通过反复抽吸并超声的方法分散于5 m L质量分数为4.0%的SBE-β-CD溶液中。色谱分离采用熔融石英毛细管色谱柱,高纯氮作载气,流速30 m L·min-（-1）,进样口温度200℃,采用程序升温,分析时间15min,氢火焰离子化检测器温度270℃。结果 1,4-丁烷磺内酯质量浓度在0.5-6 mg·L-（-1）内线性关系良好（r=0.999 3）,平均回收率在100.4%-101.5%内,精密度的RSD为4.4%,分散液液微萃取的富集因子约为12。结论该方法可用于测定SBE-β-CD样品中杂质1,4-丁烷磺内酯的限量。

A sensitive liquid chromatography and tandem mass spectrometry (LC–MS/MS) method was developed and validated for the simultaneous analysis of 15 flavonoids and 3 phenolic acids in Herba Lysimachiae and Herba Desmodii Styracifolii. Separation was performed using a Diamonsil C18 column, which was eluted with methanol (A) and 0.1‰ acetic acid (B). The gradient condition was as follows: 0–34min, 20–34% A; 34–38min, 34–95% A; maintained 95% A for the next 4min. Analytes were detected using a hybrid quadrupole linear ion trap mass spectrometer that was equipped with an electrospray ionisation source in the negative ion and multiple-reaction monitoring modes. A full validation of the method was performed, including the linearity, precision, and accuracy, as well as limits of detection and quantification. The results indicated that the developed method was simple, sensitive and reliable. Furthermore, the method was successfully applied to differentiate 16 batches of Herba Lysimachiae and 21 batches of Herba Desmodii Styracifolii.

建立了高效毛细管电泳-间接UV法测定药用辅料磺丁基醚-B-环糊精(SBE-β-CD).采用未涂层熔融石英毛细管柱,以30 mmol/L苯甲酸-三羟甲基氨基甲烷(Tris)(pH 7.5)为运行缓冲液,分离电压30 kV,检测波长214 nm.考察了缓冲液类型与pH、检测波长、电压、温度和样品浓度对测定的影响,并评价了不同批次的SBE-β-CD.