高效液相色谱法测定舒普深中的舒巴坦钠和头孢哌酮钠

 应用反相高效液相色谱外标定量法同时测定了舒普深中的舒巴坦钠和头孢哌酮钠。采用 pH 4 0的磷酸水溶液 乙腈 (体积比为 80∶2 0 )组成的流动相 ,在ODS柱上 ,于 12min内同时测定舒巴坦钠和头孢哌酮钠。方法简单 ,重现性好 ,在线性范围内舒巴坦钠的相关系数为 0 9997(n =5 ) ,头孢哌酮钠的相关系数为 0 9991(n=5 )。方法适于对药品舒普深的生产过程及临床上该药的血药浓度的监测。     

Theoretical studies of sulbactam: Reactions after acylation

DFT methods were used on the model molecular to determine the mechanism of β‐lactamase inhibitor. The results show that the thiazole ring can be opened as well as β‐lactam ring. The thiazole ring‐open product can be formed via β‐lactam ring‐open product or tetrahedral intermediate directly. Those products, in imine or enamine form, can tautomerize via hydrogen migration. The sulforious form products may be transformed into sulfonyl ones. Water or hydroxyl group in residues on active site will help lower the activation energy of above reactions, and if structure permitted, they also effect the route selection of whole reaction system. © 2007 Wiley Periodicals, Inc. Int J Quantum Chem, 2007     

Determination of cefoperazone and sulbactam in serum by HPLC‐MS/MS: An adapted method for therapeutic drug monitoring in children

A rapid, accurate and specific high‐performance liquid chromatography–tandem mass spectrometry method has been validated for the simultaneous determination of cefoperazone and sulbactam in a small volume sample for children. A Shim‐pack XR‐ODS C₁₈ column with gradient elution of water (0.1% formic acid) and acetonitrile (0.1% formic acid) solution was used for separation at a flow rate of 0.3 mL/min. The calibration curves of two analytes in serum showed excellent linearity over the concentration ranges of 0.03–10 μg/mL for cefoperazone, and 0.01–3 μg/mL for sulbactam, respectively. This method involves simple sample preparation steps and was validated according to standard US Food and Drug Administration and European Medicines Agency guidelines in terms of selectivity, linearity, detection limits, matrix effects, accuracy, precision, recovery and stability. This assay can be easily implemented in clinical practice to determine concentrations of cefoperazone and sulbactam in children.     

高效液相色谱法同时检测乳制品中3种β-内酰胺酶抑制剂的残留量

建立了乳制品中3种β-内酰胺酶抑制剂克拉维酸钾、他唑巴坦和舒巴坦的提取和固相萃取净化方法。样品经水溶后,用丙酮沉淀蛋白质。上清液在弱酸性条件下用PWAX固相萃取小柱(60 mg/3 mL)富集、净化,0.05%(如无特殊说明均为体积分数)氨水-甲醇溶液洗脱。然后采用高效液相色谱-二极管阵列检测器(HPLC-PAD)分离检测。分析柱为资生堂CAPCELL PAK MG-C18(150 mm×4.6 mm,5μm);流动相为0.03%磷酸-乙腈。该方法对克拉维酸钾、他唑巴坦和舒巴坦的最低检测质量浓度均为0.03 mg/L;纯牛奶、酸奶和奶粉中的回收率在84.6%~101.7%之间,RSD在2.2%~7.4%之间(n=6);在0.05~5 mg/L范围内均呈良好的线性关系,线性回归系数r>0.999。该方法的前处理净化效果好、检测灵敏度高、回收率和重现性良好,适用于乳制品中β-内酰胺酶抑制剂的测定。     

亲水作用色谱-串联四极杆质谱测定液态奶中舒巴坦

建立了亲水作用色谱-串联四极杆质谱测定液态奶中微量舒巴坦的分析方法。样品经0.2%乙酸水溶液提取,HLB固相萃取柱净化、富集,以甲酸铵-乙腈为流动相,经Acquity UPLC BEH HILIC色谱柱分离后采用电喷雾质谱多反应监测方式(MRM)扫描,外标法定量。结果表明,舒巴坦的质量浓度在1～100μg/L范围内线性关系良好,r2大于0.99,定量下限为1.0μg/kg。加标水平在1.0～50.0μg/kg范围时,回收率为82%～102%,相对标准偏差(RSD)为1.6%～4.7%。该方法前处理简便快捷、灵敏度高、回收率和重现性良好,适用于液态奶中舒巴坦的测定。     

Simultaneous determination of rifampicin and sulbactam in mouse plasma by high-performance liquid chromatography

A simple and rapid high-performance liquid chromatographic (HPLC) method with ultraviolet detection has been developed and validated for the simultaneous determination of rifampicin and sulbactam in mouse plasma. Plasma samples were deproteinized with acetonitrile and separated by HPLC on a RP-18 (125 x 4 mm, 5 microm) column and gradient elution with potassium dihydrogen phosphate solution (pH 4.5; 50 mm) and acetonitrile at a flow-rate of 1.0 mL/min. Rifampicin and sulbactam were monitored at 230 nm and confirmed by means of their UV spectra using a diode-array detector. The method was linear at plasma levels from 1 to 100 microg/mL for rifampicin and from 5 to 200 microg/mL for sulbactam. The limits of quantification were 0.6 microg/mL for rifampicin and 4.2 microg/mL for sulbactam. The intra- and inter-day precisions of the method (RSD) were lower than 5% for both compounds. Average recoveries of rifampicin and sulbactam from mice plasma were 98.2 and 89.3%, respectively. The developed method was successfully applied to the determination of the pharmacokinetic profile of both compounds in mice.