实验模拟氧化条件对微生物四醚脂的环境替代指标的影响

以古菌和细菌细胞膜脂甘油四烷基甘油四醚(GDGTs)为基础建立的古温度指标四醚指数(TEX86)与甲基化/环化指标(MBT/CBT),以及陆源输入指标(BIT)与干旱和盐碱化指标Ri/b,在海洋、湖泊、黄土-古土壤等沉积物的古环境重建中得到了广泛的应用.然而,利用这些微生物分子指标来重建古环境时,氧化等降解因素对GDGTs化合物,尤其是对细菌支链GDGTs的影响目前还不是很清楚.本研究通过过氧化氢模拟不同氧化程度对土壤中GDGTs化合物产生的影响,进而分析古菌和细菌GDGTs不同结构化合物抗氧化能力的差异,了解化学氧化降解对GDGTs各指标的影响.结果表明,古菌类异戊二烯GDGTs抗氧化能力低于细菌支链GDGTs,同时含环的古菌和细菌GDGTs抗化学氧化能力均要低于无环GDGTs.古菌GDGTs古温度指标TEX86在氧化过程中逐渐降低,在氧化条件下沉积的古菌GDGTs的TEX86指标用于古温度的重建存在低估的可能.在以无环细菌支链GDGTs为主的环境中,细菌MBT/CBT指标随氧化程度加深其重建温度基本不受影响.古菌与细菌GDGTs抗降解能力的差异导致陆源输入指标BIT指数随着氧化程度增加而升高,在地质体中应用此指标恢复古陆源输入存在高估的可能性.干旱化和盐碱化指标Ri/b随着氧化程度加深表现出逐渐降低的趋势,从而在应用上也可能存在低估.需要指出的是,实验室用的过氧化氢比自然条件下氧气的氧化作用强得多,本文的结论反映了一种比较极端的状况.     

示踪全球环境变化的微生物代用指标

文章详细总结了示踪全球环境变化的一系列微生物替代指标。重建古温度的定量指标包括藻类长链烯酮的U、古菌甘油二烷基甘油四醚化合物(GDGTs)的TEX_(86)指标、细菌GDGTs的甲基化指数(MBT)与环化指数(CBT)的组合。古温度的定性指标有脂类单体的氢同位素组成、不饱和脂肪酸的相对含量、有孔虫和硅藻的组合及其生物体的同位素组成和微量元素比值。重建古水文的指标包括有壳变形虫组合、细菌GDGTs的环化指数CBT、细菌和古菌GDGTs的陆源输入指数BIT、古菌和细菌GDGTs的相对丰度R、直链脂肪族化合物的碳优势指数CPI、好氧与厌氧微生物的丰度。古大气CO_2分压的估算可采用藻类长链烯酮的碳同位素组成、有孔虫的硼同位素组成。认为这些微生物指标在古环境重建中潜力巨大,并对一些重要微生物指标的应用原理和限定条件进行了分析。有些指标因受多种环境因子和成岩作用的影响,在应用中需特别的注意,不能无限夸大其应用领域。     

西沙地区碳酸盐台地发育过程与海平面变化:基于西科1井BIT指标分析数据

为了探讨南海碳酸盐台地的发育过程及控制因素, 采用有机分子化合物指标方法对其进行了研究.有机分子化合物指标BIT(branched isoprenoid tetraether)是沉积物中源自陆源的细菌膜脂支链甘油双烷基链甘油四醚(branched glycerol dialkyl glycerol tetraethers,简称bGDGTs)与主要来自海洋泉古菌中的类异戊二烯GDGTs(isoprenoid GDGTs,简称iGDGTs)的含量之比,在古环境研究中,用来区分沉积物有机质的来源、判断沉积环境.通过对西科1井的数据研究发现,西科1井BIT指数随深度呈现三段式规律性变化,从下到上呈现高-低-高的变化,反映了中中新世以来南海海平面变化及碳酸盐台地生长发育的过程:在中中新世晚期,受全球及区域海平面变化下降影响,西沙地区碳酸盐台地形成礁-滩交互的沉积地层,由于大气淡水的影响,造成BIT指数呈现高值;到晚中新世至上新世,全球及区域海平面出现持续上升,有利于西沙碳酸盐台地的生长发育,使该井沉积环境以礁内泻湖相为主,造成BIT指数呈现低值;在第四纪冰期,全球及区域海平面出现总体下降趋势,西沙碳酸盐台地又频繁暴露于地表,造成BIT指数又呈现高值.研究表明,西沙地区碳酸盐台地受区域相对海平面变化影响更大,说明南海海平面变化既受全球海平面变化的影响,也受南海区域构造沉降的控制.      

GDGTs温度指标在青藏高原湖泊的应用潜力分析——以昆仑山黑海为例

古温度的定量重建已成为理解地球气候系统演化的关键性环节,然而目前可靠的陆地温度重建指标仍然较少。来源于微生物细胞膜的甘油二烷基甘油四醚膜类脂（GDGTs）及其相关指标（甲基化/环化指标MBT/CBT和四醚指标TEX86）在湖泊古温度的定量重建中具有一定的潜力,但由于湖泊系统的复杂性及高原气候的特殊性等问题,使得相关指标在青藏高原湖泊的应用受到影响。因此,对目标湖泊开展详细的现代过程分析,考察GDGTs温度指标的应用潜力尤为重要。以位于藏北高原的黑海作为研究对象,采集表层沉积物、流域土壤以及入湖河流沉积物共24个样品。分析了黑海沉积系统中GDGTs的来源,探讨了GDGTs及其相关指标对环境因子的响应,考察了MBT/CBT指标及温度转换函数在高原湖泊温度重建中的适用性。结果表明：黑海中存在部分内源性GDGTs;水体深度对GDGTs的组成与分布影响较显著,电导率与总有机碳的影响较弱;MBT/CBT指标在高海拔和寒冷地区的湖泊古温度重建中有一定的局限性,应该结合区域特点、气候类型及母源微生物对特殊环境的生态响应等,建立更加适用于高原湖泊的温度指标及校正方程。     

微生物四醚膜脂化合物在湖泊环境中的研究进展

近十几年来,甘油二烷基甘油四醚类化合物(GDGTs)已成为生物地球化学研究的热点,此类化合物广泛分布在海洋、湖泊、土壤、泥炭以及热泉等不同类型的环境载体中,并且携带丰富的环境信息,基于此类化合物分布构建的参数已成为重建古环境变迁的重要指标。本文首先从GDGTs化合物的结构以及生物来源出发,重点阐述了基于此类化合物构建的几个指标TEX86、BIT、MBT/CBT以及ACE在湖泊环境研究中的应用及存在的不足,随后概述了特殊类型湖泊即富营养、高盐度湖泊中GDGTs化合物的分布特征,最后对GDGTs化合物在湖泊环境的研究提出总结以及展望。     

地质环境中生物标志物GDGTs分析技术研究进展

甘油二烷基甘油四醚脂（GDGTs）是一类来自于微生物细胞膜脂的新兴生物标志物,广泛存在于海洋、湖泊、土壤、泥炭等环境。在活体细胞中,GDGTs通常以完整极性膜脂（IPL-GDGTs）的形式存在,而在地质环境中主要以脱去极性头基的核心脂（CL-GDGTs）的形式存在。CL-GDGTs结构稳定、不易降解,并且对环境变化响应敏感,因此被认为是重建古气候-古环境变化的有力工具。GDGTs结构复杂、种类多样,在环境中的含量通常较低且常与其他化合物共存,因此分析难度较高,现有技术和方法在其分离、纯化、定量等方面仍然面临挑战。本文总结了近年来GDGTs在分析技术方面的研究进展,概述了GDGTs的分类与结构,对环境中IPL-GDGTs和CL-GDGTs的分离、纯化等方法进行总结和比较,其中CL-GDGTs可选择多种提取方法,而极性较强、热稳定性较差的IPL-GDGTs应尽量选取Bligh-Dyer提取法。普通的分离、纯化通常采用柱层析法,而涉及GDGTs单体分离时,一般采用制备液相色谱法。液相色谱-质谱、核磁共振波谱、气相色谱-同位素比值质谱是GDGTs含量测定、结构鉴定、同位素分析的主要分析手段。本...     

东海和黄海沉积物中海洋自生来源对支链四醚类化合物的贡献

近些年,支链甘油二烷基甘油四醚类脂物(brGDGTs)被广泛应用于陆地古气候、古环境重建研究中,并取得了一系列的进展。brGDGTs在海洋沉积物中普遍存在,起初被认为是陆源输入的结果,但越来越受到质疑。在中国东海和黄海区域,brGDGTs的相关研究还相对较少。本文分析了位于南黄海和东海北部的4个站位年龄跨度近百年的柱状岩芯,讨论了brGDGTs相关参数的特点,在此基础上探讨了brGDGTs的来源。结果显示,岩芯沉积物中brGDGTs分布样式与已发表的黄河和长江流域土壤中brGDGTs分布样式存在显著差别,暗示了海洋微生物自生brGDGTs的存在。在假设岩芯沉积物中brGDGTs主要由长江和黄河流域土壤输入和海洋微生物自生三端元贡献的情况下,用四甲基brGDGTs百分含量(%tetra)和四甲基环化指数(#Ring_(tetra))参数计算了三个端元的相对贡献和绝对变化情况。结果表明海洋自生是沉积物中brGDGTs的主要贡献者,在南黄海中北部可达70%以上。从百余年来的沉积序列来看海洋自生brGDGTs的含量有增加的趋势,这种趋势可能与海水的富营养化增强有关,也可能是随沉积深度增加降解加强的结果。     

广西南丹石炭系黄龙组下段碳酸盐岩地球化学特征及其古沉积环境意义

广西南丹大厂石炭系黄龙组碳酸盐岩对探讨右江盆地石炭系古沉积环境和古海水氧化还原特征具有重要的意义。本文对研究区碳酸盐岩样品进行全岩地球化学分析,结果显示:碳酸盐岩的Mn/Sr值均小于3,表明样品能够反映原始海相化学性质;Si O₂、Al₂O₃和Ti O₂等陆源元素的平均含量低,Zr、Th的含量较低且与∑REE相关性不明显、Y/Ho值变化大但Nd含量相对稳定,说明样品受到陆源碎屑影响有限;碳酸盐岩的Ce异常,揭示了样品形成于次氧化环境,δEu接近于现代海水值,反映样品基本不受热液活动影响。根据古水深、古气候、古盐度等特征元素指标综合判别,研究区黄龙组下段沉积期为离岸距离相对较近的浅水沉积环境,总共经历了2次相对较大的海侵和海退旋回,但海水总体呈下降趋势,整体上属温暖潮湿的气候。这也进一步反映了石炭纪右江盆地为海相沉积环境。     

安徽宣城红土微生物GDGTs分布特征及其古环境意义

中国南方更新世红土是古气候环境变化研究非常重要的载体之一,红土微生物类脂分子是其古气候环境研究的有效指标,但其在红土中的古气候意义需要更进一步的挖掘和明确.选取处于气候变化敏感地带并且已有很好年代学基础的安徽宣城红土剖面进行详细的野外调查和系统的样品采集,利用改善后的碱式水解法提取红土微生物类脂分子,通过对比分析、比较印证等方法对其中的甘油二烷基链甘油四醚(glycerol dialkyl glycerol tetraethers,简称GDGTs)进行系统研究.宣城剖面GDGTs分布特征显示:剖面下部各指标呈旋回性变化、而上部相对稳定,表明形成初期环境比较动荡,而后期成土环境相对稳定;土壤pH为7.0~8.0,推测其物源主要来源于北方干旱区或长江中下游干涸河滩沉积;BIT指标反映宣城地区在130 ka BP左右气候极为干旱.结果表明,红土中微生物类脂物GDGTs能够定量、高分辨率地重建安徽宣城的古气候环境,具有重要的研究意义.      

重庆石柱二叠纪栖霞组地球化学特征及其环境意义

在对重庆市石柱县二叠纪栖霞组地层野外露头沉积特征研究的基础上,结合室内薄片观察,根据碳酸盐岩样品的元素含量、比值及相关性,探讨了栖霞组沉积地球化学特征与古环境意义.用于古环境分析的10件栖霞组样品SiO₂、MgO含量低,且两者具有较好的正相关性,Sr含量高,平均为1 751×10-6,Mn/Sr<0.1,Fe/Sr<1,δ18O_PDB>-10‰,表明成岩过程中样品几乎不受硅化及白云岩化作用的影响,未发生化学性质上的改变,可作为古环境分析的可靠对象.栖霞组碳酸盐岩CaO含量高,平均为53.81%,接近纯灰岩的理论化学组成,陆源元素Al₂O₃、TiO₂含量很低,平均值分别为0.17%与0.012%,表明其形成于陆源碎屑影响微弱的稳定古海洋环境.古气候指标MgO/CaO比值极低,平均为0.026,古盐度指标100×(MgO/Al₂O₃)比值高,平均为1 241,古水深判别指标Sr/Ba、1000×(Sr/Ca)比值高,平均值分别为286和4.54,指示了栖霞组碳酸盐岩为潮湿气候下的陆表海(远岸)沉积.古氧相地球化学指标U/Al、V/Al、Mo/Al、Cr/Al、Co/Al、V/(V+Ni)和U/Th特征一致表明栖霞组碳酸盐岩沉积于贫氧—缺氧环境.垂向上,陆源元素∑(Al₂O₃+TiO₂)含量逐渐降低,古水深指标Sr/Ba、1000×(Sr/Ca)比值逐渐增大,表明栖霞组沉积过程中离岸渐远、陆源供给逐步减少、水体持续加深.     

Peatland GDGT records of Holocene climatic and biogeochemical responses to the Asian Monsoon

Branched and isoprenoidal glycerol dialkyl glycerol tetraether (GDGT) membrane lipids have been widely used to reconstruct past climate and environmental change. They are not, however, widely applied to peat deposits and the controls on their distributions in peats remain unclear. Here, we present a high resolution record of branched and isoprenoid GDGT concentrations and distributions from a peat core from the Tibetan Plateau that spans the last 13 kyr, a period characterised by distinct dry and wet periods in the region. The lowest concentrations of total branched glycerol dialkyl glycerol tetraethers (brGDGTs) occurred during a presumably dry interval in the mid-Holocene, suggesting that brGDGTs-producing bacteria are less productive under such conditions, perhaps reflecting their putative anaerobic ecology. The mean annual air temperature (MAT) estimates derived from the methylation index of brGDGTs and cyclisation ratio of brGDGTs (MBT′/CBT) are higher than present mean annual temperature in the region and closer to summer temperatures, perhaps due to seasonal production of brGDGTs. The downcore distributions of isoprenoidal and branched GDGTs are dominated by GDGT-0 and brGDGT II, respectively. The high fractional abundances of GDGT-0 in warm and especially wet intervals suggest that these conditions are favourable for some groups of methanogenic archaea. The mid-Holocene dry interval is associated with an increase in the fractional and absolute abundance of crenarchaeol, which could be indicative of enhanced ammonia-oxidising archaeal-mediated nitrogen cycling under these conditions. Taken together, variations of GDGT concentrations in peats appear to document the response of microbial processes to climate change and variations in the biogeochemical environment.     

Distribution of intact and core GDGTs in marine sediments

We conducted a survey of archaeal GDGT (glycerol dibiphytanyl glycerol tetraether) distributions in marine sediments deposited in a range of depositional settings. The focus was comparison of two pools presumed to have distinct geobiological significance, i.e. intact polar GDGTs (IP GDGTs) and core GDGTs (C GDGTs). The former pool has been suggested to be related to living communities of benthic archaea in marine sediments, while the latter is commonly interpreted to consist of molecular fossils from past planktonic archaeal communities that inhabited the surface ocean. Understanding the link between these two pools is important for assessment of the validity of current molecular proxies for sedimentary archaeal biomass and past sea surface temperatures. The relative distributions of GDGTs in the two pools in a core at a CH₄ rich site in the Black Sea provide evidence for in situ production of glycosidic IP GDGTs and their subsequent degradation to corresponding C GDGTs on timescales that are short in geological terms. In addition, we monitored the relationship between the IP GDGT and C GDGT pools in a sample set from various ocean basins with subseafloor depth from a few cm to 320 m and 0 to 4 Myr in age. Notable differences between the two pools can be summarized as follows: the GDGT with acyclic biphytanes, GDGT-0, and its analogues with two and three cyclopentane moieties (GDGT-2 and -3) are generally more abundant in the pool of IP GDGTs, while crenarchaeol tends to be more abundant in the C GDGT pool. Consequently, the ring index is generally higher for the C GDGTs while TEX₈₆, a molecular proxy ratio not considering the two major GDGTs, tends to be higher in the IP GDGT pool. These differences in the proportion of individual GDGTs in the two pools are probably due to in situ production of IP GDGTs with distributions differing from those of C GDGTs. Despite these differences, we observed significant correlation of these two ratios between the two pools. Specifically, in both pools TEX₈₆ is high in sediments from warm oceanic regimes and low in cold regimes. We discuss these relationships and suggest that recycling of core GDGTs by benthic archaea is an important mechanism linking both molecular pools.     

Origins of archaeal tetraether lipids in sediments: Insights from radiocarbon analysis

Understanding the supply and preservation of glycerol dibiphytanyl glycerol tetraethers (GDGTs) in marine sediments helps inform their use in paleoceanography. Compound-specific radiocarbon measurements of sedimentary alkenones from multiple environments have been used to gain insight into processes that affect paleotemperature reconstructions. Similar analyses are warranted to investigate how analogous processes affecting GDGTs impact TEX₈₆ paleotemperatures. Here we present radiocarbon measurements on individual GDGTs from Bermuda Rise and Santa Monica Basin sediments and discuss the results in the context of previous studies of co-depositional alkenones and foraminifera. The ¹⁴C contents of GDGTs and planktonic foraminifera in Bermuda Rise are very similar, suggesting a local source; and TEX₈₆-derived temperatures agree more closely with foraminiferal temperatures than do temperatures. In contrast, GDGTs in Santa Monica Basin are depleted in ¹⁴C relative to both alkenones and foraminifera, and TEX₈₆ temperatures agree poorly with known surface water values. We propose three possible factors that could explain these results: (i) GDGTs may be labile relative to alkenones during advective transport through oxic waters; (ii) archaeal production deep in the water column may contribute ¹⁴C-depleted GDGTs to sediments; and (iii) some GDGTs also may derive from sedimentary archaeal communities. Each of these three processes is likely to occur with varying relative importance depending on geographic location. The latter two may help to explain why TEX₈₆ temperature reconstructions from Santa Monica Basin do not appear to reflect actual sea surface temperatures. Terrigenous GDGTs are unlikely to be major contributors to Bermuda Rise or Santa Monica Basin sediments, based on values of the BIT index. The results also indicate that the crenarchaeol regioisomer is governed by processes different from other GDGTs. Individual measurements of the crenarchaeol regioisomer are significantly depleted in ¹⁴C relative to co-occurring GDGTs, indicating an alternative origin for this compound that presently remains unknown. Re-examination of the contribution of crenarchaeol regioisomer to the TEX₈₆ index shows that it is a significant influence on the sensitivity of temperature reconstructions.     

Differential degradation of intact polar and core glycerol dialkyl glycerol tetraether lipids upon post-depositional oxidation

Archaeal and bacterial glycerol dialkyl glycerol tetraether lipids (GDGTs) are used in various proxies, such as TEX₈₆ and the BIT index. In living organism, they contain polar head groups (intact polar lipids – IPLs). IPL GDGTs have also been detected in ancient marine sediments and it is unclear whether or not they are fossil entities or are part of living cells. In order to determine the extent of degradation of IPL GDGTs over geological timescales, we analyzed turbidite deposits, which had been partly reoxidized for several kyr after deposition on the Madeira Abyssal Plain. Analysis of core lipid (CL) and IPL-derived GDGTs showed a reduction in concentration by two orders of magnitude upon post-depositional oxidation, while IPL GDGTs with a mono- or dihexose head group decreased by 2–3 orders of magnitude. The BIT index for CL- and IPL-derived GDGTs increased substantially upon oxidation from 0.1 to up to 0.5. Together with changing MBT/CBT values, this indicates preferential preservation of soil-derived branched GDGTs over marine isoprenoid GDGTs, combined with in situ production of branched GDGTs in the sediment. The TEX₈₆ value for IPL-derived GDGTs decreased by 0.07 upon oxidation, while that of CL GDGTs showed no significant change. Isolation of IPLs revealed that the TEX₈₆ value for monohexose GDGTs was 0.55, while the that for dihexose GDGTs was substantially higher, 0.70. Thus, the decrease in TEX₈₆ for IPL-derived GDGTs was in agreement with the dominance of monohexose GDGTs in the oxidized turbidite, probably caused by a combination of in situ production as well as selective preservation of terrestrial isoprenoid GDGTs. Due to the low amount of IPL GDGTs vs. CL GDGTs, the impact of IPL degradation on CL-based TEX₈₆ paleotemperature estimates was negligible.     

Intact Polar and Core Tetraether Lipids in Sediments from the Haiyang 4 Cold-seep of the Northern South China Sea and their Implications

A number of cold seeps have been discovered in the northern South China Sea (SCS) including the Haiyang 4 cold-seep area where Core 973-5 was collected. Intact polar lipids (IPLs) and core lipids (CLs) were analyzed separately in sediments from Core 973-5. The most abundant lipid biomarkers were isoprenoidal GDGTs (isoGDGTs), with Crenarchaeol and GDGT-0 predominating. IPL-isoGDGTs and CL-isoGDGTs were mainly derived from Thaumarchaeota. IPL-isoGDGTs were mainly produced and retained in situ thus containing most of the in situ microbiological information. Branched GDGTs were predominantly derived from generated in marine production, and mixed with some terrestrial inputs. All IPLs groups presented a high value in the sulfate-methane transition zone (SMTZ). Furthermore, IPL and CL-MI, IPL-R0/4 showed the highest values within the SMTZ, while IPL and CL-R4/i had the lowest values at the SMTZ, suggesting that the contribution of Methanophila and methanogenic to GDGTs increased, while the contribution of ammonia-oxidizing Archaea to GDGTs decreased at the SMTZ.     

Stable hydrogen isotope measurement of archaeal ether-bound hydrocarbons

Compound-specific hydrogen isotope analysis of ether-bound isoprenoid hydrocarbons from archaeal membranes has been developed using chemical degradation and gas chromatography/pyrolysis/isotope ratio mass spectrometry. The ether-bound hydrocarbons are quantitatively converted to saturated hydrocarbons by cleavage of ether bonds with HI followed by H₂ reduction in the presence of PtO₂. The δD value of ether-bound hydrocarbon moieties are corrected by way of isotopic mass balance calculation for the hydrogen incorporated during the hydrogenation. The method was successfully applied to determination of the δD values of biphytane moieties in glycerol dialkyl glycerol tetraethers (GDGTs) from a Sulfolobus sp. culture and a marine sediment.     

http://www.sciencedirect.com/science/article/pii/S1674987111001332

Isoprenoidal glycerol dialkyl glycerol tetraethers（iGDGTs） from the Gulu hot springs （23-83.6℃,pH>7） and Yangbajing hot springs（80—128℃,pH>7） were analyzed in order to investigate the distribution of archaeal lipids among different hot springs in Tibet.A soil sample from Gulu was incubated at different temperatures and analyzed for changes in iGDGTs to help evaluate whether surrounding soil may contribute to the iGDGTs in hot springs.The sources of bacterial GDGTs（bGDGTs） in these hot springs were also investigated.The results revealed different profiles of iGDGTs between Gulu and Yangbajing hot springs. Core iGDGTs and polar iGDGTs also presented different patterns in each hot spring.The PCA analysis showed that the structure of polar iGDGTs can be explained by three factors and suggested multiple sources of these compounds.Bivariate correlation analysis showed significant positive correlations between polar and core bGDGTs.suggesting the in situ production of bGDGTs in the hot springs.Furthermore,in the soil incubation experiment,temperature had the most significant influence on concentration of bGDGTs rather than iGDGTs.and polar bGDGTs had greater variability than core bGDGTs with changing temperature.Our results indicated that soil input had little influence on the composition of GDGTs in Tibetan hot springs. On the other hand,ring index and TEX₈₆ values were both positively correlated with incubation temperature, suggesting that the structure of archaeal lipids changed in response to varying temperature during incubation.     

Comparison of instrumental and GDGT-based estimates of sea surface and air temperatures from the Skagerrak

Sea surface temperatures (SSTs) and annual mean air temperatures (MATs) are estimated for the last 200 years from glycerol dialkyl glycerol tetraethers (GDGTs) proxies in a marine sediment core from the Skagerrak, off southern Norway. The reconstructed values compare well with annual SSTs and summer air temperatures obtained from composite regional instrumental records. The results provide further confidence in the application of proxies based on GDGTs to estimate past temperatures.     

Separation of core and intact polar archaeal tetraether lipids using silica columns: Insights into living and fossil biomass contributions

Intact polar lipids (IPLs) are frequently used as biomarkers for living microbial cells and can be separated from core lipids (i.e. lipids without polar headgroups), which are mainly derived from fossil (i.e. dead) cell material, using column chromatography. We have compared the effect of various silica column conditions on the separation and recovery of archaeal glycerol dialkyl glycerol tetraether (GDGT) core lipids, glycolipids and phosphoglycolipids using authentic standards and direct analysis with various high performance liquid chromatography-mass spectrometry (HPLC-MS) techniques. The commonly used procedure to separate these compound classes using dichloromethane, acetone and methanol as eluents, respectively, did not separate core GDGTs from glyco- and phosphoglyco-GDGTs. In contrast, a recently described procedure using hexane:ethyl acetate (3:1, v:v), ethyl acetate and methanol achieved both high recovery and successful separation of core GDGTs from the other IPLs. Application of the method to a geothermally heated soil and suspended particulate matter from the North Sea showed that it separates most of the core GDGTs from the other IPLS and that considerable qualitative and quantitative differences can occur between core and IPL-GDGTs. We conclude that the method is therefore appropriate for the separation of intact archaeal IPLs and their fossil analogues.