Selective Identification of Organic Iodine Compounds Using Liquid Chromatography-High Resolution Mass Spectrometry.

A method to selectively and sensitively detect organic iodine compounds and identify their structures has been developed using liquid chromatography-high resolution mass spectrometry (LC-HRMS). Using extracted ion chromatograms of product ions (iodine ion) collected on a rapid scanning quadrupole orbitrap mass spectrometer, the retention times of the unknown organic iodine compounds were determined, and the structural information were acquired according to the MS/MS experiments and the matching with reference standards. We have demonstrated the application of this method by identifying unknown organic iodine compounds in seaweed. A total of 28 possible organic iodine peaks were discovered, among them, the accurate mass and element composition of the corresponding precursor ions were identified for 12 peaks, and molecular structures were confirmed for 4 peaks, which were 3-iodo-L-tyrosine, 3,5-diiodo-L-tyrosine, 4-iodophenol, and 2-iodobenzoic acid. This method is expected to lead to the future discovery of new organic iodine compounds via LC-HRMS in different environmental samples, which is crucial for understanding the iodine biogeochemical cycling.

In situ Identification of Labile Precursor Compounds and their Short-lived Intermediates in Plants using in vivo Nanospray High-resolution Mass Spectrometry.

INTRODUCTION: Many secondary metabolites in plants are labile compounds which under environmental stress, are difficult to detect and track due to the lack of rapid in situ identification techniques, making plant metabolomics research difficult. Therefore, developing a reliable analytical method for rapid in situ identification of labile compounds and their short-lived intermediates in plants is of great importance. OBJECTIVE: To develop under atmospheric pressure, a rapid in situ method for effective identification of labile compounds and their short-lived intermediates in fresh plants. METHODOLOGY: An in vivo nanospray high-resolution mass spectrometry (HR-MS) method was used for rapid capture of labile compounds and their short-lived intermediates in plants. A quartz capillary was partially inserted into fresh plant tissues, and the liquid flowed out through the capillary tube owing to the capillary effect. A high direct current (d.c.) voltage was applied to the plant to generate a spray of charged droplets from the tip of the capillary carrying bioactive molecules toward the inlet of mass spectrometer for full-scan and MS/MS analysis. RESULTS: Many labile compounds and short-lived intermediates were identified via this method: including glucosinolates and their short-lived intermediates (existing for only 10 s) in Raphanus sativus roots, alliin and its conversion intermediate (existing for 20 s) in Allium sativum and labile precursor compound chlorogenic acid in Malus pumila Mill. CONCLUSION: The method is an effective approach for in situ identification of internal labile compounds and their short-lived intermediates in fresh plants and it can be used as an auxiliary tool to explore the degradation mechanisms of new labile plant compounds. Copyright © 2016 John Wiley & Sons, Ltd.

Rapid in situ identification of bioactive compounds in plants by in vivo nanospray high-resolution mass spectrometry.

A method for the rapid in situ identification of bioactive compounds in fresh plants has been developed using in vivo nanospray coupled to high-resolution mass spectrometry (HR-MS). Using a homemade in vivo nanospray ion source, the plant liquid was drawn out from a target region and ionized in situ. The ionized bioactive compounds were then identified using Q-Orbitrap HR-MS. The accurate mass measurements of these bioactive compounds were performed by full-scan or selected ion monitoring (SIM), and tandem mass spectrometry (MS/MS) was used in the structural elucidation. Without sample pretreatment, 12 bioactive compounds in 7 different plant species were identified, namely, isoalliin in onion; butylphthalide in celery; N-methylpelletierine, pelletierine, and pseudopelletierine in pomegranate; chlorogenic acid in crabapple; solamargine, solasonine, and solasodine in nightshade; aloin and aloe-emodin in aloe; and menthone in mint. This work demonstrates that in vivo nanospray HR-MS is a good method for rapid in situ identification of bioactive compounds in plants.