Data on investigation of metabolomics and ionomics of Humulus lupulus grown in India

Abstract

The article reports data on chemical profiling of aqueous, methanolic, and n-hexane extract of field cultivated male Humulus lupulus using liquid chromatography-mass spectrometry (LC-MS) and gas chromatography-mass spectrometry (GC-MS). Also, the elemental profiling of the soil was carried out using Inductively coupled plasma mass spectrometry (ICP-MS). The elemental analysis revealed the soil to be rich in iron, calcium, magnesium, sodium, and potassium while trace elements like copper, cobalt, zinc, and molybdenum comparatively were found to be in lesser amounts. The diverse catalogues of compounds, identified in plant extracts, belong to different phytocompound groups, including phenolics, flavonoids, fatty acids, and alcohol derivatives. The compounds, such as Trans-2-methyl-4-n-pentylthiane, 2-Azido-2,4,4,6,6,8,8-heptamethylnonane were identified (with a similarity score > 65) in n-hexane, while compounds like Arsenous acid, tris(trimethylsilyl) ester and (Tris(tert-butyldimethylsilyloxy) arsane were identified in methanolic extract. The aqueous extract revealed compounds such as 2-Amino-1,3,4-octadecanetriol and Safingol with the highest peak area run in positive mode while Oleanolic acid and Gingerol have the highest peak area run in negative mode. The suggestive association between soil elemental composition, abiotic factors and plant germplasm, on phytochemical profile is proposed.

Specifications Table

Subject	Biology
Specific subject area	Medicinal plants and pharmacology.
Type of data	Raw data, Tables, Figures, Chromatograms, Text files,
Data collection	The leaves of the field-cultivated male Humulus lupulus plant (germinated from seeds) were collected, dried, and extracted in solvents like hexane, methanol, and distilled water. The GC-MS of the extracts (methanol, hexane) was carried out at Agilent 5977B EI/CI MSD (California, United States) and LC-MS of aqueous extract was carried out at Dionex Ultimate 3000, Thermo Scientific (Massachusetts, United States). The elemental analysis of the soil in which the plant propagated was carried out by ICP-MS using Agilent Technologies make Model: 7900 (California, United States).
Data source location	The seeds of Humulus lupulus were procured from Palm Beach, Europe. The seeds were potted at Jaypee Institute of Information Technology, Noida, Uttar Pradesh, India, Latitude- 28.630111° and Longitude-77.373969°. The plant propagated were used for carrying out the studies.
Data accessibility	Repository name: Mendeley Data- https://data.mendeley.com/ Data identification number: doi:10.17632/chz389f8dd.1 Direct URL to data: https://data.mendeley.com/datasets/chz389f8dd/1 Data Citation: Singh, Tripti; Mathur, Ashwani (2024), “Data on Investigation of Metabolomics and Ionomics of Humulus lupulus grown in India ”, Mendeley Data, V1, doi:10.17632/chz389f8dd.1.

1. Value of the Data

• •Hops (Humulus lupulus) have widely been explored since decades, for the plethora of phytocompounds and their reported application in therapeutics including anti-cancerous, anti-inflammatory, antioxidant, and antimicrobial properties. The plant is also effective in the treatment of metabolic syndrome and different ailments related to anxiety, stress, and sleep disorders.
• •The predictive compounds identified in the plant viz-viz in different solvents provide a direction to the researchers for exploring the therapeutic potential of the investigated compounds and suggest the role of abiotic parameters including soil properties, in regulating phytocompound biosynthesis.
• •The data obtained by different chromatography techniques may be utilized for the isolation of these compounds and their bioactivity assessment which may be further extended toward prevention of different diseases and the designing of rationalized drugs.
• •Also, the elemental profiling data would help in studying the potential correlation between plant germplasm, abiotic variables, and soil on phytochemical profile.

2. Background

Humulus lupulus, sister species of the cannabaceae family has been well known for its application in the brewing industry [1]. The plant is rich in secondary metabolites and is well known for treatment of metabolic syndrome and has also been explored for its therapeutic potential down the lane [[2], [3], [4]]. The genetic factors play a pivotal role in controlling the metabolic profiling of the medicinal plants however their production is also influenced to some extent by the environmental factors [5]. Different abiotic environmental factors like demography (latitude and longitude), climatic conditions, intensity of light, edaphic variations and interactions among the biotic components influences the amount and content of phytochemicals present in the plant. The degree of variation and adaptation to particular environmental factors may be reflected in the association between the level of secondary metabolites and external variables [[6], [7], [8], [9], [10], [11]]. Thus, the present study deals with the investigation of the metabolic and elemental profiling of Humulus lupulus, a plant of medicinal benefit grown in India.

3. Data Description

The plant Humulus lupulus is propagated via seeds at JIIT premises (Fig. 1). The present data pertains to predictive compounds identified in methanolic and n-hexane extracts of Humulus lupulus using GC-MS as shown in Table 1 (raw data 3 and 4). The compounds identified has been compared with NIST library and the comparative chromatograms have been depicted in Table 2. The compounds in the aqueous extract were screened using LC-MS and the data is presented in Table 3 (raw data 1 (negative mode) and 2 (positive mode)). The concentration of the elements present in the soil sample was analyzed using ICP-MS (raw data 5) and the data is shown in Table 4.

Fig. 1.

Humulus lupulus propagated at JIIT premises.

Table 1.

Predictive secondary metabolites identified in n-hexane and methanolic extract of Humulus lupulus using gas chromatography-mass spectroscopy.

Solvent	Compound Name	PubChem ID	MW (g/mol)	Molecular Formula	Similarity Score
Hexane	Propanoic acid, 2,2- dimethyl-, anhydride with diethylborinic acid	546082	170.06	C9H19BO2	61.30
	Borinic acid, diethyl	522516	99.97	C4H11BO	63.37
	2-Azido-2,4,4,6,6-pentamethylheptane	546203	211.35	C12H25N3	64.37
	Trans-2-methyl-4-n-pentylthiane	12680844	218.356 Da	C11H22S	67.00
	Benzene, 1,3-bis(1,1-dimethylethyl)	136810	190.32	C14H22	68.20
	2,4-Di-tert-butylphenol	7311	206.32	C14H22O	60.02
	Trihexadecyl borate	292409	735.1	C48H99BO3	61.32
	2-Azido-2,4,4,6,6,8,8-heptamethylnonane	546206	267.45	C16H33N3	69.65
Methanol	Arsenous acid, tris(trimethylsilyl) ester	180508	342.49	C9H27AsO3Si3	72.74
	Benzoic acid 1-methoxy-1H-tetrazol-5-ylmethyl ester	569263	234.21	C10H10N4O3	42.40
	trans-2,4-Dimethylthiane, S,S-dioxide	71394538	130.25	C7H14S	53.02
	(Tris(tert-butyldimethylsilyloxy)arsane	91733954	468.7	C18H45AsO3Si3	65.77

Table 2.

Comparative table for observed and library spectra of compounds detected in n-hexane and methanolic extract of Humulus lupulus using GC-MS.

Table 3.

Predictive secondary metabolites identified in aqueous extract of Humulus lupulus using liquid chromatography-mass spectroscopy.

Mode Type	Compound Name	Molecular Formula	Molecular Weight	m/z	Area
Positive	2-Amino-1,3,4-octadecanetriol	C18 H39 NO3	317.29	318.2	2,214,830,943.58
Positive	Safingol	C18 H39 NO2	301.29	302.30	2,490,302,591.78
Positive	Absinthin	C30H40O6	496.28	497.28	324,769,236.0
Positive	Kaempferol	C15 H10O6	286.04	287.05	156,569,469.34
Negative	Oleanolic acid	C30 H48O3	456.36	455.35	408,603,118.28
Negative	(+)-[6]-Gingerol	C17 H26O4	294.18	293.17	292,681,908.77
Negative	Genistein	C15 H10O5	270.05	269.04	124,081,235.20
Negative	Azelaic acid	C9 H16O4	188.10	187.09	97,740,853.97

Table 4.

Concentration of elements identified in soil sample tested using Inductively coupled plasma-mass spectrometry (ICP-MS).

Elements Name	Symbol	Atomic Mass	Atomic Number	Concentration (µg/g)
Sodium	Na	22.990	11	2635.705
Magnesium	Mg	24.305	12	8421.201
Phosphorus	P	30.974	15	2831.709
Potassium	K	39.098	19	10,562.468
Calcium	Ca	40.078	20	15,626.745
Manganese	Mn	54.938	25	970.605
Iron	Fe	55.845	26	41,739.123
Cobalt	Co	58.933	27	9.570
Copper	Cu	63.546	29	45.279
Zinc	Zn	65.38	30	215.144
Molybdenum	Mo	95.95	42	1.510

4. Experimental Design, Materials and Methods

4.1. Collection of plant material and preparation

The seeds of Humulus lupulus were procured from Palm Beach (Europe). The seeds were propagated in the soil at Jaypee Institute of Information Technology, Noida, Uttar Pradesh, India. Once the plant was propagated the plant specimen was identified by the Department of Forest Products at DR Y.S. Parmar University of Horticulture & Forestry, Nauni, Solan (Himachal Pradesh), India. The leaves were harvested during the vegetative phase of plant growth. The collected leaves were washed and kept on air drying.

4.2. Plant sample extraction

The dried leaves were crushed using a mortar and pestle and were mixed with different solvents viz. n-hexane, methane, and distilled water respectively. The mixtures were kept on shaking (Tarsons, India) for 48 h at 100 rpm around 30 °C. After 48 hrs the samples were filtered using whatman paper and kept for drying. The supernatant of the plant was kept on drying and scraped using a spatula. Stock concentrations of (5mg/mL) were made and dilutions (1mg/mL) were used for carrying out GC and LC-MS. The soil sample was collected from the field and dried for ICP-MS to be carried out.

4.3. Liquid chromatography/mass spectroscopy (LC-MS)

The LC-MS of the samples were carried out as method reported by Singh and Mathur with modifications [12]. The LC-MS analysis was conducted on Dionex Ultimate 3000, Thermo Scientific (Massachusetts, United States) equipped with Q Exactive, Thermo Scientific. The Hypersil Gold C18 with dimensions 2.1 mm x 100 mm, 3.0 µm used was to inject the sample volume of 15 µl at a flow rate of 0.350 mL/min. The machine was run in both modes (Positive (+), Negative (-) with a scan range of 120–800 m/z and capillary voltage of (+) 3.5 kV to (-) 2.5 kV respectively. The raw data was analyzed using the software ThermoFisher Scientific Compound Discoverer 3.3.

4.4. Gas chromatography/mass spectroscopy (GC-MS)

The GC-MS analysis was carried out at Agilent 5977B EI/CI MSD (California, United States). 10 µl of the sample was injected in the column with a flow rate of 1.21 mL/min. The GC-MS was carried out as method reported by Srivastava and Mathur with modifications [13]. The injection temperature was maintained at 260 °C with a pressure of 90.5 kPa. The instrument temperature was increased initially from 100 °C to 300 °C. The MS start and end times were 4.0 and 39.9 min while the start and end times of m/z were 40 and 600 respectively. The sample spectra were compared with NIST library for predictive compound identification with a similarity score.

4.5. Inductively coupled plasma/mass spectroscopy (ICP-MS)

The ICP-MS of the samples were carried out using method reported by Trimmel et al. with modifications [14]. The digestion of the samples was carried out at Microwave Reaction System (Anton Paar make model: Multiwave PRO) (Graz, Austria). 8 mL of nitric acid was used to digest the sample, and volume was added up to 40 mL. The samples were filtered using a 0.2-micron membrane. For ICP-MS the samples were tested on Agilent Technologies, Model: 7900 (California, United States). The He gas flow was set at 0.2 mL/min with both the nebulizer and auxillary gas flow rate of 1 L/min.

Limitations

Not applicable.

Ethics Statement

The authors have read and followed the ethical requirements for publication in Data in Brief confirming that the current work does not involve human subjects, animal experiments, or any data collected from social media platforms.

CRediT Author Statement

Tripti Singh: Conceptualization, Methodology, Data Curation, Investigation, Writing- Original draft preparation. Ashwani Mathur: Visualization, Supervision, Validation, Writing- Reviewing and Editing.

Data Availability

• Mendeley DataData on Investigation of Metabolomics and Ionomics of Humulus lupulus grown in India (Original data)