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. 2025 Jul 29;14(15):2336. doi: 10.3390/plants14152336

Chemical Composition and Acaricidal Activity of Lantana camara L. Essential Oils Against Rhipicephalus microplus

Jorge Ramírez 1,*, Karla Balcázar 2, Jéssica López 2, Leydy Nathaly Castillo 1, Ruth Ortega 3, Haydee Vidal López 4, Ernesto Delgado-Fernández 5, Wilmer Vacacela 4, James Calva 1, Chabaco Armijos 1
Editor: William N Setzer
PMCID: PMC12348604  PMID: 40805685

Abstract

For the first time, essential oils (EOs) from the leaves and flowers of Lantana camara L., grown in Loja, Ecuador, have been isolated by steam distillation and analyzed. The oil yields from the extractions were 0.021 and 0.005% for the leaves and flowers, respectively. A compositional analysis using gas chromatography revealed the presence of EOs, comprising approximately 97.98% of the extract from the leaves and 74.58% of the extract from the flowers. The chemical characterization of these EOs indicated sesquiterpenic profiles. The most representative constituents of the essential oils from the flowers were γ-Curcumene (21.79%), (E, E)-α-Farnesene (20.07%), and α-Zingiberene (13.38%), while the EOs from the leaves were characterized by the abundant presence of γ-Curcumene (21.87%), (E)-Nerolidol (15.09%), and cis-Muurola-4(14),5-diene (12.65%). Furthermore, the acaricidal efficacy of the EOs from the leaves of L. camara was tested by a dip test with adult ticks, resulting in acaricidal efficacy at concentrations of 10%, demonstrating the useful properties of these EOs.

Keywords: acaricidal efficacy, chemical composition, essential oil, GC-MS, Lantana camara, Rhipicephalus microplus

1. Introduction

The Verbenaceae family has 100 genera and approximately 2600 species, with the vast majority distributed in Latin America [1]. The best-known genera in this family are Aloysia, Caryopteris, Citharexylum, Clerodendrum, Duranta, Lantana, Petrea, Stachytarpheta, Phyla, Verbena, and Vitex [2,3]. Lantana has approximately 80 species distributed in tropical and subtropical America; these species are recognized for their ethnomedicinal, pharmaceutical, and ornamental uses [4]. Lantana camara is one of the most relevant species within this genus, commonly known in Ecuador as five blacks, holy blacks, seven colors, royal sage, supirosa, or venturosa [5]. This species, globally recognized as an ornamental plant, exhibits aromatic, small, and multicolored flowers. Its foliage consists of perennial, serrated, oval, and pubescent leaves. The plant typically ranges in height from 1 to 4 m and demonstrates a significant reproductive capacity, yielding up to 12,000 fruits annually [6,7]. L. camara has been used to treat and prevent pathologies, including cancer [8]. Its leaves are used for digestive and respiratory problems. Its root is used to purify the blood as well as for liver diseases [9]. In the same way, its infusion is used to treat tumors, measles, malaria and other health problems such as toothache, kidney issues, and digestive issues including diarrhea, vomiting, and flatulence. Other uses include treating burns, diabetes, pimples, and pangs [10,11,12].

Verbenaceae are well recognized for the presence of compounds, such as thymol, β-caryophyllene, citral, 1,8-cineole, carvona, and limonene, which are capable of modifying the permeability of the bacterial membrane, causing synergism with antibiotics and preventing the development of certain microorganisms without producing toxic effects [13]. Ecuador, recognized as a biodiverse nation, possesses a wealth of plant resources. However, despite this significant diversity, ethnomedicinal and phytotherapeutic research aimed at fully exploiting the properties of its flora remains limited. Consequently, there is a growing interest in conducting studies to identify the chemical composition of various native species [14].

Considering that essential oils (EOs) are the ideal prototype to be used as a raw material destined for different uses by the industry [15,16], and given that, until now, there have been no reports about the effects of L. camara derivatives on ticks, this work aimed to evaluate the acaricidal effects of the EOs obtained from L. camara against the common cattle tick Rhipicephalus (Boophilus) microplus. Taking into account that EOs are a promising source of naturally occurring bioactive compounds that show acaricide/insecticide activities, we hope that this work will be of interest to the scientific community in the field of natural products.

2. Results

2.1. Essential Oil Isolation

EOs of L. camara were obtained by steam distillation, with extraction yields of 0.021% (v/w) from the leaves and 0.005% (v/w) from the flowers.

2.2. Chemical Analysis of Essential Oils

GC-MS and GC-FID analyses of L. camara EOs showed that hydrocarbon sesquiterpenes were the primary constituents of the chemical profile, accounting for 97.98% of the identified compounds of the leaf oils and 74.58% of the flower oils. As the principal components of leaves, the EOs are listed and shown in Figure 1: γ-Curcumene (1) (21.87 ± 0.10), (E)-Nerolidol (2) (15.09 ± 0.07), cis-Muurola-4(14),5-diene (3) (12.65 ± 0.20), Camphene (4) (5.63 ± 0.12), p-Mentha-1(7),8-diene (5) (4.91 ± 0.09), (E)-Caryophyllene (6) (4.29 ± 0.02), α-Humulene (7) (4.23 ± 0.02), α-Phellandrene (8) (3.69 ± 0.07), Myrcene (9) (2.93 ± 0.04), and β-Curcumene (10) (2.79 ± 0.02). In the flowers’ EOs, the more abundant components were γ-Curcumene (1) (21.79 ± 0.68), (E,E)-α-Farnesene (11) (20.07 ± 1.36), α-Zingiberene (12) (13.38 ± 0.33), β-Curcumene (10) (5.34 ± 0.20), α-Humulene (7) (5.26 ± 0.16), Sclarene (13) (3.65 ± 2.68), and β-Elemene (14) (2.99 ± 0.57). Both chemical profiles obtained in this study are detailed in Table 1, the gas chromatograms of EOs are available Supplementary Material.

Figure 1.

Figure 1

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Chemical structures of the main components of the EOs of L. camara from Ecuador.

Table 1.

Chemical composition of the essential oils from leaves and flowers of Lantana camara L.

No. Compound LRI a LRI b Leaves Flowers
% ± SD % ± SD
1 Sabinene 961 969 0.19 ± 0.00 -
2 Camphene 966 946 5.63 ± 0.12 -
3 δ-2-Carene 977 1001 0.16 ± 0.00 -
4 Verbene 980 961 0.03 ± 0.00 -
5 α-Phellandrene 993 1002 3.69 ± 0.07 0.12 ± 0.01
6 p-Mentha-1(7),8-diene 997 1003 4.91 ± 0.09 0.35 ± 0.03
7 Pentyl propanoate 1001 1005 1.28 ± 0.02 -
8 Myrcene 1005 988 2.93 ± 0.04 -
9 3-Octanol 1015 988 0.11 ± 0.00 -
11 α-Terpinene 1028 1014 0.10 ± 0.00 -
12 ο-Cymene 1032 1022 0.05 ± 0.00 -
13 Sylvestrene 1038 1025 1.12 ± 0.02 0.21 ± 0.02
14 1,8-Cineole 1042 1026 0.84 ± 0.01 -
15 (Z)-β-Ocimene 1045 1032 0.04 ± 0.00 -
16 (E)-β-Ocimene 1053 1044 0.51 ± 0.01 -
17 γ-Terpinene 1064 1054 0.33 ± 0.00 0.56 ± 0.02
18 cis-Sabinene hydrate 1078 1065 0.06 ± 0.05 -
19 Terpinolene 1089 1086 0.14 ± 0.11 -
20 Linalool 1106 1095 0.54 ± 0.01 -
21 n-Nonanal 1113 1100 0.07 ± 0.00 -
22 α-Fenchocamphorone 1116 1104 0.05 ± 0.00 -
23 trans-Pinocarveol 1146 1135 0.06 ± 0.00 -
24 cis-Verbenol 1148 1137 0.12 ± 0.00 -
25 trans-Verbenol 1153 1140 0.24 ± 0.00 -
26 Borneol 1179 1165 0.07 ± 0.01 -
27 Terpinen-4-ol 1186 1174 0.24 ± 0.01 -
28 α-Terpineol 1203 1186 0.30 ± 0.00 -
29 (3Z)-Hexenyl 3-methyl butanoate 1236 1232 0.08 ± 0.00 -
30 (2Z)-Hexenyl isovalerate 1242 1241 0.09 ± 0.00 -
31 Methyl citronellate 1249 1257 0.06 ± 0.00 -
32 Geranial 1279 1264 0.04 ± 0.00 -
33 trans-Pinocarvyl acetate 1300 1298 0.14 ± 0.00 -
34 δ-Elemene 1335 1335 0.23 ± 0.01 0.66 ± 0.23
35 α-Terpinyl acetate 1353 1346 0.08 ± 0.00 -
36 Eugenol 1364 1356 0.07 ± 0.00 -
37 Cyclosativene 1369 1369 0.03 ± 0.00 -
38 α-Copaene 1375 1374 0.28 ± 0.00 0.63 ± 0.28
39 β-Bourbonene 1383 1387 0.20 ± 0.01 0.33 ± 0.03
40 β-Cubebene 1388 1387 0.27 ± 0.00 -
41 β-Elemene 1390 1389 1.86 ± 0.12 2.99 ± 0.57
42 α-Funebrene 1402 1402 0.57 ± 0.00 0.97 ± 0.03
43 Italicene 1405 1405 0.01 ± 0.00 0.05 ± 0.02
44 α-Cedrene 1416 1410 0.28 ± 0.00 0.47 ± 0.01
45 (E)-Caryophyllene 1419 1427 4.29 ± 0.02 -
46 β-Ylangene 1424 1419 0.05 ± 0.00 -
47 cis-Thujopsene 1428 1429 0.39 ± 0.00 0.66 ± 0.02
48 β-Copaene 1431 1430 0.77 ± 0.03 -
49 β-Gurjunene 1431 1431 - 1.25 ± 0.18
50 α-trans-Bergamotene 1434 1432 0.03 ± 0.00 -
51 Aromadendrene 1439 1439 0.06 ± 0.00 0.55 ± 0.04
52 2-epi-β-Funebrene 1443 1411 0.32 ± 0.01 -
53 transMuurola-3,5-diene 1448 1451 0.03 ± 0.00 -
54 cis-Cadina-1(6),4-diene 1450 1461 0.10 ± 0.01 -
55 α-Humulene 1457 1452 4.23 ± 0.02 5.26 ± 0.16
56 Amorpha-4,11-diene 1459 1449 0.30 ± 0.01 -
57 9-epi-(E)-Caryophyllene 1461 1464 0.13 ± 0.01 -
58 α-Acoradiene 1468 1464 0.07 ± 0.00 0.01 ± 0.05
59 α-Neocallitropsene 1470 1474 0.20 ± 0.00 -
60 Dauca-5,8-diene 1474 1471 - 0.46 ± 0.05
61 γ-Muurolene 1475 1478 0.18 ± 0.00 -
62 cis-Muurola-4(14),5-diene 1484 1465 12.65 ± 0.20 -
63 ar-Curcumene 1485 1479 1.28 ± 0.02 -
64 Viridiflorene 1494 1496 0.10 ± 0.00 -
65 α-Zingiberene 1497 1493 - 13.38 ± 0.33
66 γ-Curcumene 1498 1481 21.87 ± 0.10 21.79 ± 0.68
67 α-Muurolene 1502 1500 0.06 ± 0.00 trace
68 cis-β-Guaiene 1506 1492 0.43 ± 0.06 -
69 β-Macrocarpene 1510 1499 - 0.47 ± 0.19
70 β-Curcumene 1513 1514 2.79 ± 0.02 5.34 ± 0.20
71 δ-Amorphene 1517 1511 0.41 ± 0.01 -
72 Cubebol 1521 1514 0.23 ± 0.00 -
73 δ-Cadinene 1522 1522 0.27 ± 0.00 0.63 ± 0.02
74 β-Sesquiphellandrene 1428 1421 0.04 ± 0.00 0.50 ± 0.02
75 trans-Calamenene 1536 1521 0.05 ± 0.00 -
76 Italicene ether 1540 1536 0.01 ± 0.00 -
77 Silphiperfol-5-en-3-ol A 1550 1557 0.02 ± 0.00 -
78 γ-Cuprenene 1559 1532 - 0.12 ± 0.01
79 trans-Dauca-4(11),7-diene 1558 1556 - 0.16 ± 0.01
80 trans-Sesquisabinene hydrate 1561 1577 0.09 ± 0.00 -
81 Germacrene B 1563 1559 1.01 ± 0.02 1.56 ± 0.07
82 (E,E)-α-Farnesene 1567 1505 - 20.07 ± 1.36
83 (E)-Nerolidol 1568 1561 15.09 ± 0.07 -
84 Spathulenol 1585 1577 0.70 ± 0.01 -
85 Caryophyllene oxide 1589 1582 0.14 ± 0.00 -
86 n-Hexyl benzoate 1589 1579 0.24 ± 0.03 -
87 Guaiol 1596 1600 0.09 ± 0.00 -
88 Viridiflorol 1601 1592 0.20 ± 0.01 -
89 Junenol 1613 1618 0.05 ± 0.00 -
90 Rosifoliol 1616 1600 0.14 ± 0.04 -
91 epi-Cedrol 1619 1618 - 0.29 ± 0.02
92 cis-Cadin-4-en-7-ol 1623 1635 - 1.62 ± 0.09
93 α-Corocalene 1628 1622 0.04 ± 0.00 -
94 Eremoligenol 1631 1629 0.07 ± 0.00 -
95 epi-α-Cadinol 1635 1638 0.24 ± 0.01 0.11 ± 0.01
96 β-Acorenol 1642 1636 0.18 ± 0.13 -
97 Himachalol 1642 1652 - 0.83 ± 0.05
98 1-epi-Cubenol 1644 1627 0.10 ± 0.14 -
99 Valerianol 1654 1656 - 0.19 ± 0.06
100 Cubenol 1654 1645 0.06 ± 0.00 -
101 epi-α-Muurolol 1656 1640 0.03 ± 0.00 -
102 α-Muurolol (Torreyol) 1659 1644 0.07 ± 0.01 0.45 ± 0.02
103 7-epi-α-Eudesmol 1659 1662 - 0.15 ± 0.04
104 α-Cadinol 1668 1652 0.08 ± 0.01 -
105 (Z)-α-Santalol 1680 1674 - 0.31 ± 0.04
106 β-Bisabolol 1680 1674 0.06 ± 0.01 -
107 11-αH-Himachal-4-en-1-β-ol 1695 1699 0.06 ± 0.01 -
108 Sclarene 1977 1974 - 3.65 ± 2.68
109 (6E,10Z)-Pseudo phytol 2034 2018 - 0.43 ± 0.14
Monoterpene hydrocarbons 19.83 1.24
Oxygenated monoterpenoids 2.58 -
Sesquiterpene hydrocarbons 58.34 65.09
Oxygenated sesquiterpenoids 15.27 3.94
Others 1.96 4.31
TOTAL 97.98 74.58
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LRI a, linear retention index calculated; LRI b, linear retention index from [17]; %, percentage; SD, standard deviation. Both values were conveyed as means of three determinations.

2.3. Acaricidal Effect of L. camara Essential Oil

The highest value of tick mortality (100%) was achieved with 10% and 15% EO L. Allmara. All results are shown in Table 2 and Table 3, respectively.

Table 2.

Mortality percentage of Rhipicephalus (Boophilus) microplus following treatment with different concentrations of Lantana camara essential oil, with olive oil as a control.

Engorged Ticks Group Treatments
Olive Oil
(1)		 10% of L. camara EO
(2)		 15% of L. camara EO
(3)
1 0 100 100
2 0 100 100
3 0 100 100
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Table 3.

Mortality percentages of Rhipicephalus (Boophilus) microplus.

Repetition Treatment No. of Ticks Exposed No. of Dead Ticks Mortality (%)
1 Olive oil (control) 10 0 0
1 10% of L. camara EO 10 10 100
1 15% of L. camara EO 10 10 100
2 Olive oil (control) 10 0 0
2 10% of L. camara EO 10 10 100
2 15% of L. camara EO 10 10 100
3 Olive oil (control) 10 0 0
3 10% of L. camara EO 10 10 100
3 15% of L. camara EO 10 10 100
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Table 2 shows the percentages of mortality observed in three distinct groups of engorged ticks subjected to varying treatments. The results indicated that Treatment 1 did not have any impact on the tested groups, while Treatments 2 and 3 resulted in 100% mortality, showing that these essential oils have strong acaricidal properties.

In Table 3, we have included specific results about the number of repetitions, treatment, ticks exposed, number of ticks dead, and mortality percentages.

2.4. ANOVA Analysis

In order to evaluate whether a significant difference existed between the mean mortality rates of the treatments, an ANOVA analysis was performed; the results are displayed in Table 4. Comparisons were conducted to visualize the statistical significance of differences in the dependent variable between the treatment control group and the remaining groups employing 10% and 15% concentrations.

Table 4.

Analysis of variance (ANOVA) of mortality percentages in Rhipicephalus (Boophilus) microplus according to treatment.

S.V S.S df MS F p-Value
Model 20,000.00 2 10,000.00 1.61 × 1016 <0.001
TTO 20,000.00 2 10,000.00 sd sd
Error 3.7 × 10−12 6 0.00
Total 20,000.00 8
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S.V = Source of variation, S.S = sum of squares, df = degrees of freedom, MS = mean square, F = F-statistic/F-ratio, p-value = probability value, Model = Statistical model, TTO = Treatment; error = Experimental error.

The results of the analysis of variance indicated a significant difference between the control treatment and the evaluated treatments; however, no statistically significant differences were found between the treatments themselves.

3. Discussion

The chemical composition of the essential oils obtained from leaves and flowers of L. camara was elucidated. Gas chromatography-mass spectrometry analysis of the essential oil identified sesquiterpene hydrocarbons, with γ-curcumene being the main compound in both compositions (leaves: 21.87 ± 0.10; flowers: 21.79 ± 0.68).

The primary constituents of the essential oil extracted from L. camara flowers have been reported in several studies undertaken across diverse geographical locations. For instance, a study in Saudi Arabia identified caryophyllene oxide (10.6%), β-caryophyllene (9.7%), spathulenol (8.6%), γ-cadinene (5.6%), and trans-β-farnesene (5.0%) as the major components [18]. In Bregbo, southeastern Côte d’Ivoire, where flowers were collected during two distinct periods, the predominant compounds were (E)-β-caryophyllene (ranging from 19.2% to 36.6%) and α-humulene (ranging from 8.5% to 19.9%) [19]. Analysis of L. camara flower essential oil from Nigeria revealed sabinene (21.5%), 1,8-cineole (12.6%), β-caryophyllene (13.4%), and α-humulene (5.8%) as the most abundant constituents [20], whereas an analysis from India determined that the essential oil was predominantly composed of β-caryophyllene (26.9%), bicyclogermacrene (12.5%), and cis-davanone (7.4%) [21].

On the other hand, studies on the leaf essential oil of L. camara have shown differing profiles. One investigation reported nerolidol (E)-isomer, (43.4%), γ-cadinene (7.6%), and α-humulene (4.9%) as the main components [22]. Subsequently, in 2012, an analysis identified 71 compounds in the leaves, with β-caryophyllene, caryophyllene oxide, and β-elemene being the three most prevalent compounds [23]. Guerrero and Pozo identified 19 compounds as part of the whole compositions, with γ-muurolene (22.23%), trans-caryophyllene (17.07%), α-humulene (12.61%), γ-elemene (9.93%), and bicyclogermacrene (6.22%) being the most abundant [24]. Variations in the chemical compositions across these investigations can be attributed to several factors, including geographic location, time of collection, environmental conditions, season, temperature, and humidity. These parameters can significantly influence the relative abundance of the identified compounds.

The acaricidal effect of L. camara essential oil was evaluated at concentrations of 10% and 15% against Rhipicephalus (Boophilus) microplus, resulting in 100% mortality of adult ticks. Other studies have also evaluated the effectiveness of L. camara EO against Rhipicephalus (Boophilus) microplus through immersion tests on adults, demonstrating its effectiveness at a concentration of 100 mg/mL, whereby it notably reduced reproductive capacity by 55.65% [25]. Similarly, the acaricidal properties and safety of several plant materials, such as Ptaeroxylon obliquum, Aloe ferox, L. camara, and Tagetes minuta, used by rural farmers to control ticks on cattle, were evaluated. L. camara extracts at a 40% concentration showed an average tick load reduction of 58%, while the other plant species evaluated did not yield effective results [26]. The effectiveness observed in the present study may be attributed to the association of different active ingredients, potentially indicating synergism between active substances that optimize the action on R. (B.) microplus. According to Bakkali et al. and Showler [27,28], the acaricidal effects of EOs are associated with their bioactive compounds, highlighting the effects of multiple compounds which may act via multiple mechanisms against ectoparasites. γ-Curcumene, the major compound present in the EOs, has already been reported to exhibit various activities, including larvicidal and tickicidal effects, as demonstrated by Guzmán et al. [29], where the obtained results suggest that this compound should be further studied as a promising acaricide against R. microplus.

The control of Rhipicephalus microplus, an ectoparasite affecting cattle production worldwide, remains a major challenge for the livestock industry. It is estimated that Rhipicephalus species affect more than 80% of the global cattle population, causing significant economic losses due to reduced milk and meat production, transmission of pathogens, and costs associated with tick control [29]. In countries like Brazil and Mexico, annual losses attributed to R. microplus infestations have been estimated al USD 3.24 billion and USD 573.6 million, respectively [30]. In Ecuador, the situation is similarly concerning, where the unregulated and excessive use of synthetic acaricides has led to environmental contamination, food safety issues, and the emergence of acaricide-resistant tick populations, as reported by local veterinarians [29]. These challenges highlight the urgent need for alternative, sustainable, and eco-friendly control methods.

Although commercial biological control products exist for the control of ticks, many of these present limitations, such as high toxicity to non-target organisms, inconsistent efficacy, or rapid development of resistance. In this context, plant-derived essential oils have gained attention due to their biodegradability, low mammalian toxicity, and multiple modes of action, which reduce the likelihood of resistance development. Essential oils, such as those extracted from Lantana camara, have shown promising acaricidal activity due to the presence of bioactive compounds like sesquiterpenes and monoterpenoids, which interfere with the nervous system of arthropods, causing neurotoxic effects, paralysis, and death [31]. These natural compounds also exhibit repellent properties, which can prevent tick attachment and feeding, making them effective tools for integrated pest management strategies [29].

Previous studies have shown that Lantana camara essential oils exhibit high toxicity against Rhipicephalus microplus larvae, achieving mortality rates exceeding 90% at concentrations of 20 mg/mL. Studies have demonstrated that the essential oils from its leaves and flowers exhibit potent acaricidal activity [31,32,33,34,35]. This oil not only affects larval stages but also inhibits egg laying and larval development, suggesting its ability to interfere with the tick’s life cycle [35]. Moreover, it has been shown to significantly reduce oviposition and egg hatching, reinforcing its potential as a biocontrol agent. These findings support the feasibility of conducting new bioassays with this essential oil, especially in regions such as southern Ecuador, where phytochemical variability could yield even more promising effects.

4. Materials and Methods

4.1. Materials and Chemical Reagents

Standard aliphatic hydrocarbons for the GC-FID calibration curve were obtained from Chem Service (Sigma-Aldrich, St. Louis, MO, USA), and helium was supplied from INDURA (Quito, Ecuador). Anhydrous sodium sulfate was purchased from Sigma-Aldrich (San Luis, MO, USA). Olive oil and 95% ethanol were bought in local supermarkets. All solvents and reagents used were of analytical grade and were employed without further purification.

4.2. Plant Material

The collection of L. camara, authorized by the Ministry of the Environment of Ecuador (MAE), N°001-IC-FLO-DBAP-VS-DRLZCH-MA, took place during the late flowering stage in the Yaguarcuna neighborhood, Loja, Ecuador (4°11′10.518″ S–79°59′48.8148″ W). Once the plant material had been collected, it was transported to the Bioproducts Plant of the Universidad Técnica Particular de Loja, where the fresh leaves and flowers were separated prior to steam distillation for essential oil extraction.

4.3. Distillation of the Volatile Fraction

A total of 9 kg of leaves and 4.5 kg of flowers were separately subjected to hydrodistillation using a stainless steel Clevenger-type stainless steel apparatus for 90 min at atmospheric pressure. After the distillation was complete, the essential oil was dried using anhydrous sodium sulfate and subsequently stored at −4 °C.

4.4. Qualitative and Quantitative Analysis of the Essential Oils

Chemical compositions of the volatile fraction were analyzed using gas chromatography coupled with mass spectrometry (GC-MS). A Thermo Fisher Scientific model Trace 1310 gas chromatograph (GC), equipped with a Thermo Scientific AI/AS 1300 autosampler and an ISQ7000 single quadrupole mass spectrometer controlled by Chromeleon 7.2 Chromatography Data System (CDS) software (Waltham, MA, USA), was employed. The mass spectrometer operated with electron ionization at 70 eV, scanning a mass range of 40–350 m/z. Helium was used as the carrier gas at a constant flow rate of 1.00 mL/min. A 1 µL sample was injected into a DB-5 ms capillary column (5% phenylmethylpolysiloxane, 30 m × 0.25 mm internal diameter, 0.25 μm film thickness). The oven temperature program started at 60 °C (held for 5 min), then increased to 200 °C at a rate of 2 °C per minute, and finally reached 250 °C at a rate of 15 °C per minute (held for 5 min). The ion source and quadrupole temperatures were maintained at 230 °C and 150 °C, respectively. Each sample was analyzed in triplicate. The amount of each volatile component was determined using gas chromatography coupled with a flame-ionization detector (GC-FID). The same analytical conditions and column as the GC-MS method were used, with a split ratio of 1:40.

Individual compounds were identified by comparing their mass spectra and linear retention indices (LRIs) based on data reported in scientific literature [17]. The LRIs were experimentally calculated using the method described by Van Den Dool and Kratz [36], by injecting a series of straight-chain alkanes (C9 to C24). The relative percentage of each identified compound was calculated based on the normalized peak area relative to the total area of all identified compounds in the chromatogram.

4.5. Evaluation of the Acaricidal Effect of the Essential Oil

The study population was 90 adult ticks of the genus Rhipicephalus (Boophilus) microplus, obtained from adult cattle from the Ceibopamba sector of the Malacatos parish of the Loja canton, which were randomly sampled. The ticks were then divided into three experimental groups with 10 observational units each, distributed for the three treatments.

4.5.1. Dip Test of Adult Ticks

This study employed a modified engorged female immersion test, based on the protocol by Drummond et al. [37] and adapted by FAO [38], to evaluate ixodicide efficacy. Engorged adult female ticks (n = 90) were subjected to different concentrations of test substances for thirty minutes, followed by seven days of incubation at 27 °C and 80–90% relative humidity. The experimental setup utilized a humidity chamber, water, a 200 mL beaker, a glass stirring rod, markers for identification, nine Petri dishes, 24-well culture plates, an incubator with controlled temperature and humidity (verified by a thermohygrometer), and labeling tape. L. camara essential oil and olive oil served as the positive and negative controls, respectively.

The experimental procedure involved an immersion bioassay of engorged female Rhipicephalus (Boophilus) microplus ticks to assess the acaricidal activity of Lantana camara essential oil (EO). A total of 90 surface-sterilized ticks (using 0.05% sodium hypochlorite, followed by rinsing and drying) were randomly assigned to three treatment groups (n = 30 ticks per group; 10 ticks per replicate). The groups were as follows: Group 1, treated with olive oil (100%) as the negative control; Group 2, treated with a 10% dilution of L. camara EO in ethanol; and Group 3, treated with a 15% dilution of L. camara EO in ethanol. Pure (undiluted) essential oil was not tested due to its high viscosity and potential for inconsistent application, as observed in preliminary trials. Each group of ten ticks was immersed in 30 mL of the respective solution for 30 min. After immersion, ticks were carefully removed using a fine mesh strainer, air-dried, and incubated under controlled conditions (27 ± 1 °C, 80% relative humidity, and a 12:12 h light:dark photoperiod). Mortality was evaluated after seven days by visually determining the proportion of dead ticks in each group [39].

4.5.2. Statistical Analysis

A completely randomized experimental design was employed to evaluate the effect of EO concentration on tick mortality across replicates, which allowed us to make a comparison between treatment and repetitions. Data were subjected to one-way analysis of variance (ANOVA) using SPSS Statistics version 29.0, and the differences were considered statistically significant at p < 0.05.

5. Conclusions

Briefly, chemical analysis of L. camara essential oil from both the leaves and flowers revealed γ-Curcumene as the predominant sesquiterpene hydrocarbon. While this finding aligns with some reports on L. camara essential oil composition, significant variations exist across geographical locations, highlighting the influence of environmental factors and collection parameters on the chemical profile of essential oils. Notably, L. camara EO and its extracts have demonstrated promising acaricidal activity against the prevalent cattle tick Rhipicephalus (Boophilus) microplus, achieving high mortality rates and reducing reproductive capacity. Given the substantial global economic impact of Rhipicephalus infestations and the limitations of conventional control methods, the demonstrated efficacy of L. camara EO, potentially attributed to the synergistic action of its bioactive compounds like γ-Curcumene, warrants further investigation through comprehensive bioassays with a multi-target mechanism. While its effect may be slower, its eco-friendly profile and potential for developing sustainable formulations make it a promising alternative, especially for regions with high resistance to synthetic compounds.

Furthermore, the results of the present work contribute to the growing body of scientific evidence about the biological activity in L. camara and their products, as reported recently [40].

Acknowledgments

We are grateful to the Universidad Técnica Particular de Loja (UTPL) for supporting this investigation and open access publication.

Supplementary Materials

The following supporting information can be downloaded at: https://www.mdpi.com/article/10.3390/plants14152336/s1.

plants-14-02336-s001.zip (155.1KB, zip)

Author Contributions

Conceptualization, J.R., R.O., H.V.L., J.C., C.A., E.D.-F. and W.V.; investigation, K.B. and J.L.; writing—original draft preparation, L.N.C. and J.R.; writing—review and editing, J.R., L.N.C. and W.V. All authors have read and agreed to the published version of the manuscript.

Data Availability Statement

The original contributions presented in this study are included in the article. Further inquiries can be directed to the corresponding authors.

Conflicts of Interest

The authors declare no conflicts of interest.

Funding Statement

This research received no external funding.

Footnotes

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Associated Data

This section collects any data citations, data availability statements, or supplementary materials included in this article.

Supplementary Materials

plants-14-02336-s001.zip (155.1KB, zip)

Data Availability Statement

The original contributions presented in this study are included in the article. Further inquiries can be directed to the corresponding authors.

Articles from Plants are provided here courtesy of Multidisciplinary Digital Publishing Institute (MDPI)

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