<?xml version="1.0" encoding="ISO-8859-1"?><article xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink" xmlns:xsi="http://www.w3.org/2001/XMLSchema-instance">
<front>
<journal-meta>
<journal-id>0121-0807</journal-id>
<journal-title><![CDATA[Revista de la Universidad Industrial de Santander. Salud]]></journal-title>
<abbrev-journal-title><![CDATA[Rev. Univ. Ind. Santander. Salud]]></abbrev-journal-title>
<issn>0121-0807</issn>
<publisher>
<publisher-name><![CDATA[Universidad Industrial de Santander]]></publisher-name>
</publisher>
</journal-meta>
<article-meta>
<article-id>S0121-08072020000300261</article-id>
<article-id pub-id-type="doi">10.18273/revsal.v52n3-2020008</article-id>
<title-group>
<article-title xml:lang="es"><![CDATA[Hallazgo de diclofenaco en un producto fitoterapéutico a base de caléndula comercializado en Colombia]]></article-title>
<article-title xml:lang="en"><![CDATA[Finding diclofenac in a marigold-based phytotherapeutic product marketed in Colombia]]></article-title>
</title-group>
<contrib-group>
<contrib contrib-type="author">
<name>
<surname><![CDATA[Stashenko]]></surname>
<given-names><![CDATA[Elena E.]]></given-names>
</name>
<xref ref-type="aff" rid="Aff"/>
</contrib>
<contrib contrib-type="author">
<name>
<surname><![CDATA[González]]></surname>
<given-names><![CDATA[Andrés F.]]></given-names>
</name>
<xref ref-type="aff" rid="Aff"/>
</contrib>
<contrib contrib-type="author">
<name>
<surname><![CDATA[Martínez]]></surname>
<given-names><![CDATA[Jairo R.]]></given-names>
</name>
<xref ref-type="aff" rid="Aff"/>
</contrib>
<contrib contrib-type="author">
<name>
<surname><![CDATA[Durán]]></surname>
<given-names><![CDATA[Camilo]]></given-names>
</name>
<xref ref-type="aff" rid="Aff"/>
</contrib>
<contrib contrib-type="author">
<name>
<surname><![CDATA[Oliveros]]></surname>
<given-names><![CDATA[Cristian]]></given-names>
</name>
<xref ref-type="aff" rid="Aff"/>
</contrib>
<contrib contrib-type="author">
<name>
<surname><![CDATA[Gualteros]]></surname>
<given-names><![CDATA[Leyde K.]]></given-names>
</name>
<xref ref-type="aff" rid="Aff"/>
</contrib>
<contrib contrib-type="author">
<name>
<surname><![CDATA[Salgar]]></surname>
<given-names><![CDATA[William]]></given-names>
</name>
<xref ref-type="aff" rid="Aff"/>
</contrib>
<contrib contrib-type="author">
<name>
<surname><![CDATA[Henríquez]]></surname>
<given-names><![CDATA[Camilo]]></given-names>
</name>
<xref ref-type="aff" rid="Aff"/>
</contrib>
<contrib contrib-type="author">
<name>
<surname><![CDATA[Rojas]]></surname>
<given-names><![CDATA[Diego]]></given-names>
</name>
<xref ref-type="aff" rid="Aff"/>
</contrib>
</contrib-group>
<aff id="Af1">
<institution><![CDATA[,Universidad Industrial de Santander  ]]></institution>
<addr-line><![CDATA[Bucaramanga ]]></addr-line>
<country>Colombia</country>
</aff>
<pub-date pub-type="pub">
<day>00</day>
<month>09</month>
<year>2020</year>
</pub-date>
<pub-date pub-type="epub">
<day>00</day>
<month>09</month>
<year>2020</year>
</pub-date>
<volume>52</volume>
<numero>3</numero>
<fpage>261</fpage>
<lpage>284</lpage>
<copyright-statement/>
<copyright-year/>
<self-uri xlink:href="http://www.scielo.org.co/scielo.php?script=sci_arttext&amp;pid=S0121-08072020000300261&amp;lng=en&amp;nrm=iso"></self-uri><self-uri xlink:href="http://www.scielo.org.co/scielo.php?script=sci_abstract&amp;pid=S0121-08072020000300261&amp;lng=en&amp;nrm=iso"></self-uri><self-uri xlink:href="http://www.scielo.org.co/scielo.php?script=sci_pdf&amp;pid=S0121-08072020000300261&amp;lng=en&amp;nrm=iso"></self-uri><abstract abstract-type="short" xml:lang="es"><p><![CDATA[Resumen  Introducción: la consulta de un particular que trajo un producto fitoterapéutico a base de caléndula cuyo consumo le causó fuertes reacciones adversas, originó esta investigación sobre la composición de este producto.  Objetivo: caracterizar la composición química de muestras de lotes diferentes de un producto comercial denominado fitoterapéutico a base de caléndula (Calendula officinalis) (PFC) comercializado en Colombia.  Metodología: se analizaron tabletas de ocho cajas del PFC de cuatro lotes diferentes de producción (2017 y 2018). Se llevó a cabo el análisis de espacio de cabeza (HS) de tabletas por microextracción en fase sólida (SPME), con una fibra PDMS/DVB (65 µm), expuesta al HS de la muestra durante 30 min a 50 °C. Las fracciones volátiles se analizaron por cromatografía de gases acoplada a espectrometría de masas (GC/MS). Los extractos de tabletas obtenidos con mezcla de metanol:agua (1:1, v/v) se analizaron por cromatografía líquida (LC) de alta (HPLC) y ultra-alta eficiencia (UHPLC), con detectores de arreglo de diodos (DAD) y espectrometría de masas de alta resolución (HRMS), respectivamente; la cuantificación de diclofenaco se hizo por calibración con patrón externo y por adición de estándar. Los espectros de masas de baja y alta resolución y patrones de fragmentación de las sustancias detectadas se estudiaron, usando GC/HRMS y LC/HRMS-Orbitrap.  Resultados: en tabletas analizadas por HSSPME, se encontraron monoterpenoides y sesquiterpenoides de origen vegetal, ftalatos, residuos de solventes (2-cloroetanol, etilenglicol) y sustancias químicas intermediarias en la síntesis de diclofenaco (2,6-dicloroanilina y 2,6-cloro-N-fenil-bencenamina). En los cromatogramas, obtenidos por GC/MS de los extractos de tabletas obtenidos con diclorometano, se detectaron diclofenaco, sus impurezas A, B y C, los ésteres de diclofenaco y algunas otras impurezas. Diclofenaco en cantidad ca. 40 mg (7-8%) se cuantificó por HPLC en tabletas (&gt; 70 analizadas) escogidas al azar de ocho cajas del PFC, adquirido en el mercado local de Bucaramanga (Colombia).  Conclusión: en cada tableta analizada se determinaron alrededor de 40 mg del compuesto sintético diclofenaco (sustancia no declarada en la etiqueta del producto) y en ninguna se detectaron ésteres de los triterpenoides oleanano o faradiol, constituyentes del extracto de caléndula que poseen actividad antiinflamatoria; se encontraron algunos flavonoides comunes a muchas plantas, en cantidades mil veces menores que la de diclofenaco.]]></p></abstract>
<abstract abstract-type="short" xml:lang="en"><p><![CDATA[Abstract  Introduction: The consultation of a person who brought a marigold-based phytotherapeutic product whose consumption caused strong adverse reactions, originated this investigation of the composition of this product.  Objective: to characterize the chemical composition of samples of different lots of a commercial product called calendula-based phytotherapeutic product (Calendula officinalis) (PFC) commercialized in Colombia.  Methodology: Tablets of eight packs of the phytotherapeutic product from four different production batches (2017 and 2018) were analyzed. Headspace analysis (HS) of tablets by solid phase microextraction (SPME) was carried out with a PDMS/ DVB fiber (65 µm), exposed to the HS of the sample for 30 min at 50 °C. Volatile fractions were analyzed by gas chromatography coupled to mass spectrometry (GC/MS). Tablet extracts obtained with methanol:water mixture (1:1, v / v) were analyzed by liquid chromatography (LC) of high (HPLC) and ultra-high performance (UHPLC) with diode array (DAD) and high-resolution mass spectrometric (HRMS) detectors, respectively; diclofenac was quantified by external calibration and standard addition. Low- and high-resolution mass spectra (MS, HRMS) and fragmentation patterns of detected substances were studied, using GC/HRTOF-MS and LC/HRMS-Orbitrap.  Results: in tablets analyzed by HS-SPME, monoterpenoids and sesquiterpenoids of plant origin, phthalates, solvent residues (2-chloroethanol, ethylene glycol) and intermediary chemicals in diclofenac synthesis (2,6-dichloroaniline and 2,6- chloro-N-phenyl-benzenamine) were found. In the chromatograms (GC/MS) of the extracts of tablets obtained with organic solvent (dichloromethane), diclofenac, its impurities A, B and C, diclofenac esters, and some other compounds were detected; diclofenac quantification by HPLC found amounts of ca. 40 mg (7 - 8%) in tablets (&gt; 70 analyzed) chosen at random from eight packs of the calendula-based phytotherapeutic product, purchased in the local market in Bucaramanga (Colombia).  Conclusion: each analyzed tablet contained around 40 mg of the synthetic compound diclofenac (substance not declared in the product&#8217;s label) and no tablet contained detectable amounts of esters of the triterpenoids oleanane or faradiol, which are calendula extract constituents that possess antiinflammatory activity; a few flavonoids that are common to many plants were found in amounts a thousand times smaller than that of diclofenac.]]></p></abstract>
<kwd-group>
<kwd lng="es"><![CDATA[Diclofenaco]]></kwd>
<kwd lng="es"><![CDATA[Fitoterapéutico]]></kwd>
<kwd lng="es"><![CDATA[Calendula officinalis]]></kwd>
<kwd lng="es"><![CDATA[GC/MS]]></kwd>
<kwd lng="es"><![CDATA[HPLC]]></kwd>
<kwd lng="es"><![CDATA[LC/MS]]></kwd>
<kwd lng="en"><![CDATA[Diclofenac]]></kwd>
<kwd lng="en"><![CDATA[Phytotherapeutic]]></kwd>
<kwd lng="en"><![CDATA[Calendula officinalis]]></kwd>
<kwd lng="en"><![CDATA[GC/MS, HPLC, LC/MS]]></kwd>
</kwd-group>
</article-meta>
</front><back>
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