Method development of levoglucosenone analysis by UHPLC-UV-MS in fast pyrolysis samples and aspects of its degradation in aqueous samples,Analytical Methods

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Method development of levoglucosenone analysis by UHPLC-UV-MS in fast pyrolysis samples and aspects of its degradation in aqueous samples
Analytical Methods ( IF 2.7 ) Pub Date : 2020-09-22 , DOI: 10.1039/d0ay01478h
D. Godina _{1,

2,

3,

4,

5} , K. Meile _{1,

2,

3} , A. Zhurinsh _{1,

2,

3} , A. Viksna _{2,

3,

4,

5}

Affiliation

Levoglucosenone ((1S,5R)-6,8-dioxabicyclo[3.2.1]oct-2-en-4-one or LGO; CAS number: 37112-31-5) is an extensively studied biomass based chemical and its potential applications in organic synthesis, as well as in the extraction of various natural substances, have been established; therefore developing dependable, yet fast and simple analytical methods for determining LGO in the products of thermochemical biomass processing is of great importance. In this work different UHPLC methods have been developed and compared for the determination of LGO in wood pyrolysis products. In addition to UV detection, LGO determination conditions by single quadrupole mass spectrometry have been adjusted with and without chemical derivatization. The ionization of LGO in the positive and negative electrospray ionisation mode and the effect of a mobile phase additive on LGO and its degradation product ionisation have been evaluated. Using the UHPLC-UV system, a method for the quantification of levoglucosenone was developed and the analytical parameters of the method were determined. Utilising the developed UHPLC-UV method, studies of LGO stability in standard solution and in fast pyrolysis products were carried out in various solvent systems at different temperatures and pH levels. The main LGO primary degradation product has been confirmed to be furfural. It has been concluded that the degradation rate of LGO is significantly affected by the solvent and storage temperature, so it is essential that LGO standard solutions and samples are analysed when freshly prepared. Using a UHPLC-MS system and derivatization with 2,4-dinitrophenylhydrazine (DNPH), a method for the determination of LGO was developed and the method analytical parameters were tested. To sum up, quantitative determination of LGO in pyrolysis products can be performed by reversed phase UHPLC-UV without any particular sample preparation, but in the case of UHPLC-MS it is necessary to derivatize LGO with DNPH to ensure ionisation of LGO. The additional work, requiring MS detection, can be outweighed by the greater selectivity compared to that of the more straightforward UV detection method in cases of incomplete chromatographic separation.

中文翻译：

UHPLC-UV-MS对快速热解样品中左旋葡糖酮进行分析的方法开发及其在水性样品中的降解方面

左旋葡糖酮（（1 S，5 R）-6,8-dioxabicyclocyclo [3.2.1] oct-2-en-4-one或LGO; 化学文摘社编号：37112-31-5）是一种经过广泛研究的以生物质为基础的化学物质，其在有机合成以及各种天然物质的提取中的潜在应用已得到确立；因此，开发可靠，快速而简单的分析方法来测定热化学生物质加工产品中的LGO至关重要。在这项工作中，已经开发了不同的UHPLC方法，并将其用于测定木材热解产物中LGO的含量。除检测紫外线外，还通过或不进行化学衍生化来调整通过单四极杆质谱法测定LGO的条件。已评估了正电喷雾和负电喷雾电离模式下LGO的电离以及流动相添加剂对LGO及其降解产物电离的影响。使用UHPLC-UV系统，开发了一种左旋葡萄糖苷的定量方法，并确定了该方法的分析参数。利用发达的UHPLC-UV方法，研究了LGO在标准溶液和快速热解产物中的稳定性，并在各种溶剂系统中于不同温度和pH值下进行了研究。LGO的主要降解产物已被证实是糠醛。已经得出的结论是，LGO的降解速率受溶剂和储存温度的影响很大，因此在新鲜制备时分析LGO标准溶液和样品至关重要。使用UHPLC-MS系统并用2,4-二硝基苯肼（DNPH）衍生化，开发了一种测定LGO的方法，并测试了该方法的分析参数。总而言之，可以通过反相UHPLC-UV进行热解产物中LGO的定量测定，而无需任何特定的样品前处理，但是在UHPLC-MS的情况下，必须用DNPH衍生化LGO以确保LGO离子化。在色谱分离不完全的情况下，与更直接的UV检测方法相比，需要进行MS检测的其他工作可能会被更大的选择性所抵消。热解产物中LGO的定量测定可以通过反相UHPLC-UV进行，而无需任何特殊的样品前处理，但是在UHPLC-MS的情况下，必须用DNPH衍生化LGO以确保LGO离子化。在色谱分离不完全的情况下，与更直接的UV检测方法相比，需要进行MS检测的其他工作可能会被更大的选择性所抵消。热解产物中LGO的定量测定可以通过反相UHPLC-UV进行，而无需任何特殊的样品前处理，但是在UHPLC-MS的情况下，必须用DNPH衍生化LGO以确保LGO离子化。在色谱分离不完全的情况下，与更直接的UV检测方法相比，需要进行MS检测的附加工作可能会比更高的选择性更具优势。

更新日期：2020-11-03

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