Identification of ubiquinones and menaquinones in activated sludge by liquid chromatography-atmospheric pressure chemical ionization mass spectrometry.
Identification of ubiquinones and menaquinones in activated sludge by liquid chromatography-atmospheric pressure chemical ionization mass spectrometry.
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液相色谱-常压化学电离质谱法鉴定活性污泥中的泛醌和甲基萘醌。
DOI：
10.1016/s0021-9673(03)00930-0
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发表时间：
2003
期刊：
影响因子：
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通讯作者：
Hongyan Li
中科院分区：
文献类型：
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作者：
M. Gao;Min Yang;Jianying Hu;B. Shao;Hai;Hongyan Li
建立了一种灵敏的液相色谱-大气压化学电离质谱负离子模式（LC-NI-APCI-MS）分析方法，用于鉴定活性污泥中的泛醌（UQ-n（Hx））和甲萘醌（MK-n（Hx））。在Sep-Pak Plus Silica固相萃取柱上进行样品的萃取和净化。采用ODS分析柱，以异丙醚-甲醇（17：83，v/v）为移动的流动相，实现了醌类化合物的完全分离。利用保留时间、分子离子质量和碎片离子质量的组合信息直接确定泛醌和甲基萘醌的组成。在SIM模式下使用LC-NI-APCI-MS，UQ-6、UQ-10和维生素K1的最低仪器定量检测限（LODinst）估计为0.4、4和0.12 ng（S/N=10），通过加标实验获得的UQ-6、UQ-10和维生素K1的最低方法检测限（LODmeth）估计为0.2、2和0.06 μg/g。分别另一方面，在全扫描模式下使用LC-NI-APCI-MS估计UQ-6、UQ-10和维生素K1的LODinsts分别为10、100和2 ng（S/N=10），UQ-6、UQ-10和维生素K1的LODmeths分别估计为7、60和1.2 μg/g。采用LC-NI-APCI-MS和LC-UV/DAD对活性污泥提取液进行分析。通过LC-NI-APCI-MS检测到UQ-n（n = 6 - 10）、MK-n（n= 6-10）、MK-n（H2）（n=7-10）、MK-n（H4）（n=8-9）和MK-8（H6），而通过LC-UV/DAD未检测到UQ-6、UQ-7、MK-7（H2）、MK-9和MK-10（H2）。这些结果表明，LC-NI-APCI-MS比LC-UV/DAD更灵敏地分析环境样品中的醌类化合物，如沉积物，活性污泥和生物过程中的生物膜和其他水生环境。
A sensitive analytical method has been developed for identification of ubiquinones (UQ-n(Hx)) and menaquinones (MK-n(Hx)) in activated sludge by liquid chromatography–atmospheric pressure chemical ionization mass spectrometry in negative mode (LC-NI-APCI-MS). Extraction and clean-up of samples were carried out on Sep-Pak Plus Silica solid-phase extraction cartridges. Complete separation of quinones was achieved with an ODS analytical column and using isopropyl ether–methanol (17:83, v/v) as the mobile phase. The compositions of ubiquinones and menaquinones were determined directly using combined information on retention time, the molecular ion mass and fragment ion masses. The lowest instrument quantitative detection limits (LODinst) for UQ-6, UQ-10, and Vitamin K1 were estimated to be 0.4, 4 and 0.12 ng (S/N=10) using LC-NI-APCI-MS in SIM mode, and the lowest method detection limits (LODmeth) achieved by spiking experiment were estimated to be 0.2, 2 and 0.06 μg/g for UQ-6, UQ-10 and Vitamin K1, respectively. On the other hand, the LODinstfor UQ-6, UQ-10, and Vitamin K1 were estimated to be 10, 100 and 2 ng (S/N=10) using LC-NI-APCI-MS in full-scan mode, and the LODmethwere estimated to be 7, 60 and 1.2 μg/g for UQ-6, UQ-10, and Vitamin K1, respectively. Both LC-NI-APCI-MS and LC–UV/DAD were applied in the analysis of an activated sludge extract. UQ-n (n=6–10), MK-n (n=6–10), MK-n(H2) (n=7–10), MK-n(H4) (n=8–9) and MK-8(H6) were detected by LC-NI-APCI-MS, while UQ-6, UQ-7, MK-7(H2), MK-9 and MK-10(H2) were not found by LC–UV/DAD. These results suggest that LC-NI-APCI-MS is more sensitive than LC–UV/DAD for the analysis of quinones in environmental samples such as sediment, activated sludge and bio-film in biological processes and other aquatic environments.
使用醌谱表征厌氧消化过程中的微生物群落
DOI：
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发表时间：
2009
期刊：
影响因子：
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作者：
Muhammad Hanif;Yoichi Atsuta and Hiroyuki Daimon
通讯作者：
Yoichi Atsuta and Hiroyuki Daimon