Bethel Christopher R, Distler Anne M, Ruszczycky Mark W, Carey Marianne P, Carey Paul R, Hujer Andrea M, Taracila Magda, Helfand Marion S, Thomson Jodi M, Kalp Matthew, Anderson Vernon E, Leonard David A, Hujer Kristine M, Abe Takao, Venkatesan Aranapakam M, Mansour Tarek S, Bonomo Robert A
Louis Stokes Cleveland Department of Veterans Affairs Medical Center, Research Service, Cleveland, Ohio 44106, USA.
Antimicrob Agents Chemother. 2008 Sep;52(9):3135-43. doi: 10.1128/AAC.01677-07. Epub 2008 Jun 16.
The partnering of a beta-lactam with a beta-lactamase inhibitor is a highly effective strategy that can be used to combat bacterial resistance to beta-lactam antibiotics mediated by serine beta-lactamases (EC 3.2.5.6). To this end, we tested two novel penem inhibitors against OXA-1, a class D beta-lactamase that is resistant to inactivation by tazobactam. The K(i) of each penem inhibitor for OXA-1 was in the nM range (K(i) of penem 1, 45 +/- 8 nM; K(i) of penem 2, 12 +/- 2 nM). The first-order rate constant for enzyme and inhibitor complex inactivation of penems 1 and 2 for OXA-1 beta-lactamase were 0.13 +/- 0.01 s(-1) and 0.11 +/- 0.01 s(-1), respectively. By using an inhibitor-to-enzyme ratio of 1:1, 100% inactivation was achieved in <or=900 s and the recovery of OXA-1 beta-lactamase activity was not detected at 24 h. Covalent adducts of penems 1 and 2 (changes in molecular masses, +306 +/- 3 and +321 +/- 3 Da, respectively) were identified by electrospray ionization mass spectrometry (ESI-MS). After tryptic digestion of OXA-1 inactivated by penems 1 and 2, ESI-MS and matrix-assisted laser desorption ionization-time-of-flight MS identified the adducts of 306 +/- 3 and 321 +/- 3 Da attached to the peptide containing the active-site Ser67. The base hydrolysis of penem 2, monitored by serial (1)H nuclear magnetic resonance analysis, suggested that penem 2 formed a linear imine species that underwent 7-endo-trig cyclization to ultimately form a cyclic enamine, the 1,4-thiazepine derivative. Susceptibility testing demonstrated that the penem inhibitors at 4 mg/liter effectively restored susceptibility to piperacillin. Penem beta-lactamase inhibitors which demonstrate high affinities and which form long-lived acyl intermediates may prove to be extremely useful against the broad range of inhibitor-resistant serine beta-lactamases present in gram-negative bacteria.
β-内酰胺与β-内酰胺酶抑制剂联合使用是一种高效策略,可用于对抗由丝氨酸β-内酰胺酶(EC 3.2.5.6)介导的细菌对β-内酰胺抗生素的耐药性。为此,我们测试了两种新型青霉烯抑制剂对OXA-1的作用,OXA-1是一种D类β-内酰胺酶,对他唑巴坦的失活具有抗性。每种青霉烯抑制剂对OXA-1的抑制常数(K(i))在纳摩尔范围内(青霉烯1的K(i)为45±8 nM;青霉烯2的K(i)为12±2 nM)。青霉烯1和2对OXA-1β-内酰胺酶的酶与抑制剂复合物失活的一级速率常数分别为0.13±0.01 s(-1)和0.11±0.01 s(-1)。使用1:1的抑制剂与酶比例,在≤900秒内实现了100%失活,并且在24小时未检测到OXA-1β-内酰胺酶活性的恢复。通过电喷雾电离质谱(ESI-MS)鉴定了青霉烯1和2的共价加合物(分子量变化分别为+306±3和+321±3 Da)。在用青霉烯1和2失活的OXA-1经胰蛋白酶消化后,ESI-MS和基质辅助激光解吸电离飞行时间质谱鉴定出306±3和321±3 Da的加合物附着于含有活性位点Ser67的肽段上。通过连续的氢核磁共振分析监测青霉烯2的碱水解,表明青霉烯2形成了一种线性亚胺物种,该物种经历7-内型-环化最终形成环状烯胺,即1,4-噻氮杂卓衍生物。药敏试验表明,4毫克/升的青霉烯抑制剂有效地恢复了对哌拉西林的敏感性。表现出高亲和力并形成长寿命酰基中间体的青霉烯β-内酰胺酶抑制剂可能被证明对革兰氏阴性菌中存在的多种耐药丝氨酸β-内酰胺酶极为有用。