Determination of phytoestrogens in dietary supplements by LC-MS/MS

Labelling data quantifying the exact content of individual phytoestrogen analytes in dietary supplements are generally poor. As these products are commonly used in the management of menopause symptoms, any clinical benefits would be dependent on the exact dosage of isoflavones received. Well-established extraction procedures and updated isotope dilution mass spectrometry liquid chromatography coupled with tandem mass spectrometry detection (LC-MS/MS) have been used to accurately quantify the concentrations of ten common isoflavones in 35 dietary supplement samples on sale in the UK, Canada and Italy. Concentration-specific ionization suppression is described for biochanin A and formononetin. All supplements contained phytoestrogens. The soya isoflavones (genistein, daidzein, glycitein) were present in all products and the majority also contained the red clover isoflavones (biochanin A, formononetin) and some the Kudzu isoflavones (daidzein, puerarin). The content of total isoflavones per dose ranged from <1 to 53 mg. Trace amounts of coumestrol were found in six products. Other less common analytes, the prenylnaringenins (6-prenylnaringenin, 8-prenylnaringenin, 6,8-diprenylnaringenin) were not found in any of the products. Only 14 of 35 supplements were found to deliver more than or equal to 40 mg day^?1 of aglycone isoflavones, a consensus dose value recognized as delivering therapeutic benefit. Eleven did not match label claims. Six delivered less than 10 mg day^?1 of isoflavones. There has been little improvement in the overall quality of industry labelling in the five years since this was last investigated. Consequently, the public, retailers and healthcare professionals should consider using standardized isoflavone supplements, which are supported by analytical measurements.     

Determination of tadalafil and N-desmethylsibutramine in health and dietary supplements using ultra-performance liquid chromatography (UPLC) coupled with quadrupole-time-of-flight mass spectrometry (Q-TOF MS)

The adulteration of dietary supplements with drugs is potentially dangerous for human health. In this study, a method was used to test simultaneously for the presence of three synthetic PDE-5 inhibitors (sildenafil, vardenafil and tadalafil), and sibutramine and its two major metabolites (N-desmethylsibutramine and N-didesmethylsibutramine) using ultra-performance liquid chromatography (UPLC) coupled with quadrupole-time-of-flight mass spectrometry (Q-TOF MS) in dietary supplements. This approach with UPLC/Q-TOF MS uses the high accurate mass of six compounds for identification and has a short run time. The recovery was from 87% to 113%; precision was less than 12.8%. The limit of detection and limit of quantification were from 0.4 to 2.0?µg?kg^?1 and from 1.3 to 6.0?µg?kg^?1, respectively. This method allows easy and fast analysis and detection of diverse adulterants.     

Isolation and identification of a sibutramine analogue adulterated in slimming dietary supplements

A suspected sibutramine analogue was detected in a slimming functional food by an ultra performance liquid chromatography–electrospray ionisation–time of flight mass spectrometry (UPLC-ESI-TOF/MS) method. The ultraviolet (UV) spectrum of this suspected compound showed close similarity to that of sibutramine. The sample was extracted with 70% MeOH and isolated by semi-preparative column chromatography. The structure of this compound was identified by spectroscopic analyses (nuclear magnetic resonance [NMR] technique, mass and tandem mass etc.). The structure of the unknown compound was demonstrated to be [(±)-dimethyl-1-[1-(3,4-dichlorophenyl)cyclobutyl]-N,N,3-trimethylbutan-1-amine (molecular formula C₁₇H₂₅NCl₂) and named as chloro-sibutramine. Compared with sibutramine, it has one more chlorine atom than the 3-cholorophenyl group so was switched to 3,4-dichlorophenyl. Until now, chloro-sibutramine was isolated for the first time from the undeclared ingredient included in dietary supplements. Although the safety of chloro-sibutramine is unknown, there is a potential health risk to consumers because of a similar skeleton to sibutramine. For public health, this sibutramine analogue has been included in the inspection list of illegal adulterants in Korea.     

Sensitive enzyme immunoassay for screening methandienone in dietary supplements

Methandienone is a synthetic exogenous steroid which, like other anabolic steroids, is strictly regulated in many countries. In recent years, increasing numbers have been detected of illegal additions into dietary supplements of methandienone and other anabolic androgenic steroids (AAS). In this work, a competitive indirect enzyme-linked immunosorbent assay (ELISA) has been constructed for the detection of methandienone using an antiserum against methandienone. Under optimal experimental conditions, the ELISA achieved a limit of detection of 0.04 ± 0.01 µg.g^?1. The obtained intra- and inter-day coefficients of variation were less than 8%. The developed ELISA was applied in the analysis of real dietary supplement samples. To minimise the effect of the sample matrix, the sample extracts were simply diluted before addition into the immunoassay. The achieved recovery values were around 100%. Results obtained from the ELISA correlated well, both in terms of accuracy and precision, with those obtained by UHPLC-MS/MS (reference method). The presented ELISA could be successfully applied for the simple screening of dietary supplements.     

Occurrence of pesticide residues and transformation products in different types of dietary supplements

The purpose of this study was to evaluate the presence of pesticide residues and transformation products in dietary supplement products. Thirty-two samples were analysed to determine 177 pesticides by gas chromatography–tandem mass spectrometry (GC-MS/MS) and 333 pesticides by liquid chromatography–high-resolution mass spectrometry (LC-HRMS). Pesticides were extracted from different kinds of dietary supplements by the use of a modified QuEChERS extraction method. Six samples contained pesticide residues at concentration up to 92.7 µg kg^?1, but only butralin exceeded the maximum residue limits set for raw material. In addition to target compounds, LC-HRMS enables the simultaneous detection of non-target pesticides. In this case, transformation products of pesticides were detected in the analysed samples using HRMS analyser (Exactive-Orbitrap). These compounds were not included in the original method, and they were monitored as post-target compounds, knowing their molecular formula and exact mass. Mass accuracy was always < 2 ppm, corresponding to a maximum mass error. The positive findings endorse the idea that a deeper and continuous investigation of pesticide residues and transformation products in dietary supplement products is necessary in order to guaranty consumer’s safety.     

Monitoring of 29 weight loss compounds in foods and dietary supplements by LC-MS/MS

Because of the rapid growth in dietary supplement availability and public concern for weight control, the investigation of foods and various dietary supplements illegally adulterated with weight loss compounds has become increasingly important. A total of 29 weight loss compounds, including sennoside, sibutramine, ephedrine and their analogues, found to be adulterated in foods and dietary supplements were simultaneously examined by LC-MS/MS. The 188 samples were collected between 2009 and 2012 in South Korea, and method validation was performed to determine the adulterants to the weight loss compounds. LODs, LOQs and linearity ranged from 0.03 to 7.5 ng ml^?1, from 0.08 to 30.00 ng ml^?1, and from 0.990 to 0.999, respectively. The results showed that nine weight loss compounds, namely bisacodyl, desmethylsibutramine, didesmethylsibutramine, ephedrine, fluoxetine, pseudoephedrine, sennoside A, sennoside B and sibutramine, were detected in 62 of all collected samples and were found in order of frequency as follows: sibutramine, 25.7%; sennoside A, 22.9%; sennoside B, 20.0%; fluoxetine, 8.6%; desmethylsibutramine, 7.1%; bisacodyl, ephedrine, and pseudoephedrine, 4.3%; and didesmethylsibutramine, 2.9%. Sibutramine, which was the most frequently found adulterant, ranged in levels from 0.03 to 132.40 mg g^?1 (2010), from 0.88 to 76.2 mg g^?1 (2011), and from 0.07 to 0.24 mg g^?1 (2012). Although the concentrations of most compounds ranged widely, some compounds such as bisacodyl and fluoxetine were found at high concentrations in several samples.     

Botanical origin authentication of dietary supplements by DNA‐based approaches

Herbal products, such as dietary supplements, have become a subject of increasing global importance for their health benefits and economic considerations. However, they have also been targets of adulteration practices, being the accurate identification of botanicals in herbal products of utmost importance to protect the health and expectations of consumers. Particularly, in the case of dietary supplements, which can have different types of formulations, the identification of plant material used in their production is often a research challenge. DNA‐based techniques have played a crucial role on the development of a wide range of tools for the authentication of herbal products. Therefore, this review intends to describe their main progresses, critically discussing their advantages and drawbacks when applied to authenticate herbal products, focusing on dietary supplements. DNA barcoding is particularly emphasized because it has provided the highest number of applications, followed by the advances on high‐resolution melting analysis combined with DNA barcodes. A special emphasis is also given to the promising approaches relying on DNA metabarcoding and isothermal amplification.     

医疗工作者膳食补充剂服用情况及认知现况调查

目的 探究疫情防控常态化下医疗工作者的膳食补充剂使用及认知情况,为医疗工作者营养支持提供思路。方法 采用方便抽样调查的方式面向2021年1—4月在鄂东医疗集团就职、参与抗击新型冠状病毒疫情的医疗工作者发放调查问卷,将回收的188份电子问卷数据采用SPSS 22.0软件进行统计分析。结果 医疗工作者总体膳食补充剂服用率为22.34%(42/188),文化程度越高、从未饮酒者的膳食补充剂服用率均显著高于文化程度低、饮酒者（P<0.05）,而服用人群和不服用人群在疲劳现况和自评健康状态并差异无统计学意义（P>0.05）;在认知态度上,服用人群在“膳食补充剂是安全的”“、膳食补充剂具有一定的健康作用”“、与药品有交互作用”这3条观点上明显持同意的态度（P<0.05）。医疗工作者主要服用的膳食补充剂前三位为复合型维生素矿物质制剂（59.52%）、单一维生素制剂（57.14%）及蛋白粉（40.48%）。Logistic回归分析结果显示,影响医疗工作者膳食补充剂服用的影响因素主要是文化程度（OR=7.314）和认为膳食补充剂是安全的支持态度上（OR=0.098）。结论 医疗工作者膳...     

Determination of non-opioid analgesics in adulterated food and dietary supplements by LC-MS/MS

Commercially available non-opioid analgesics such as acetaminophen and non-steroidal anti-inflammatory drugs (NSAIDs) have been used to adulterate some foods and dietary supplements. Considering the rapid growth of the dietary supplement market, it is essential to analyse various analgesics used for adulteration over a time period. Acetaminophen and 16 NSAIDs used to adulterate food and dietary supplements were simultaneously determined by LC-MS/MS. The method was validated by determining the coefficient of determinations, limit of quantification and recovery, and samples were analysed for the determination of analgesics. Consequently, acetaminophen, diclofenac, ibuprofen, indomethacin, naproxen and piroxicam were detected in 53 samples (n = 214). Ibuprofen was the most commonly used adulterant, which was detected in a wide concentration range (1.06–233.40 mg g^–1) and was present in about one-third of the adulterated samples. Various types of samples, in particular pills and capsules (73.6% of the total positive samples), were found to be adulterated with non-opioid analgesics. Samples containing high concentrations of analgesics can have a deleterious effect on human health, and thus the continued monitoring of adulterated food and dietary supplements is essential to maintain a healthy life.     

Reduction of blood lead levels in lead-exposed mice by dietary supplements and natural antioxidants

BACKGROUND: Lead exposure is a global environmental problem that induces lifelong adverse health effects. Our aim was to investigate the effect of dietary supplements and natural antioxidants on blood lead levels (BLL) in lead‐exposed mice, and observe their impact on the absorption of calcium, iron and zinc in vivo. RESULTS: All of selected dietary supplements (calcium lactate, zinc sulfate, ferrous sulfate, ascorbic acid and calcium‐rich milk) and natural antioxidants (extract of Chinese wolfberry, extract of Hangzhou white chrysanthemum and antioxidant extract of bamboo leaves) have promising capacity of reducing BLL in lead‐exposed mice with an reduction range from 56.2% to 65.1%. The metal ion‐mediated chelating and competitively inhibitory mechanisms may elucidate their reduction effect. Besides, blood calcium, iron and zinc levels were not significantly changed in all of the experimental groups, indicating that the intake of all additives does not disturb the absorption of essential mineral elements in mice. CONCLUSION: All the studied additives not only effectively reduce BLL, but also maintain normal calcium, iron and zinc absorption in mice. The formulation of calcium, iron and zinc supplements and/or polyphenol and vitamin‐rich antioxidants may constitute an important secondary prevention effort to reduce BLL and lead exposure. Copyright © 2010 Society of Chemical Industry     

Occurrence of aflatoxins in milk thistle herbal supplements

Milk thistle (MT) dietary supplements are widely consumed due to their possible liver-health-promoting properties. As botanicals they can be contaminated with a variety of fungi and their secondary metabolites, mycotoxins. The aflatoxigenic fungus Aspergillus flavus has been previously isolated from these commodities. Currently, there is no published method for determining aflatoxins (AFs) in MT. Therefore, a liquid chromatography (LC) method validated for aflatoxin analysis in botanicals was evaluated and applied to MT. The method consisted of acetonitrile/water extraction, immunoaffinity column clean-up, LC separation, post-column photochemical reaction derivatisation and fluorescence detection. The average recoveries for AFs added to MT seeds, herb, oil-based liquid extract and alcohol-based liquid extract were 76% or higher. The mean relative standard deviation was <10%. The limit of detection (LOD) was 0.01?µg kg^?1 and the limit of quantification (LOQ) was 0.03?µg kg^–1. The method was used to conduct a small survey. A total of 83 MT samples from the US market were analysed. AFs were detected in 19% of the samples with levels ranging from 0.04 to 2.0?µg kg^–1. Additionally, an aflatoxigenic A. flavus strain from ATTC and an A. parasiticus strain isolated from MT herb powder were found to produce high amounts of aflatoxins (11,200 and 49,100?µg kg^–1, respectively) when cultured in MT seed powder. This is the first study reporting on aflatoxin contamination of MT botanical supplements and identifying methodology for AF analysis of these commodities.     

Determination of 26 anti-diabetic compounds in dietary supplements using a validated UPLC method

The purpose of this study was to validate a rapid, simple and accurate method using ultra-performance liquid chromatography (UPLC) for the simultaneous determination of 26 anti-diabetic compounds in illegally adulterated dietary supplements. The method was validated for specificity, linearity, limit of detection, limit of quantitation, precision, accuracy, recovery and stability. All compounds were separated with a resolution of over 1.5. The limits of detection and quantitation were 0.10–1.70 and 0.30–5.10 µg g^–1 in a solid sample, respectively; the corresponding values were 0.10–1.25 and 0.30–3.75 µg ml^–1 in a liquid sample. The correlation coefficient was > 0.99, precisions were 0.11–3.30% (intra-day) and 0.05–6.15% (inter-day), and accuracies were 83–108% (intra-day) and 85–109% (inter-day). The recoveries were measured with six dosage forms, and the results were acceptable as 87–117% with relative standard deviations ≤ 6.44%. The relative standard deviations of stability were ≤ 3.40% and the standard solution was stable for 48 h. Ninety-six samples were obtained from on/off-line markets and were analysed using the developed method. Among these samples, pioglitazone and glibenclamide were found in seven samples and the concentrations of each compound were 0.15% and 0.26–0.51%, respectively. With the increasing adulteration of dietary supplements with anti-diabetic drugs, this method may be helpful to protect public health and safety.     

Detection of adulteration of anti-hypertension dietary supplements and traditional Chinese medicines with synthetic drugs using LC/MS

A sensitive and specific liquid chromatography-electrospray ionization mass spectrometry (LC/ESI-MS) method was developed for the analysis of 18 drugs used for the treatment of anti-hypertension, including diuretics, calcium antagonists, and angiogenesis-converting enzyme inhibitors (ACEI) as adulterants in dietary supplements and traditional Chinese medicines. Separation was accomplished on a Xtimate? C₁₈ reversed-phase column using a mixture of methanol, acetonitrile and 20 mM ammonium formate buffer (pH 3.2) as mobile phase. The method demonstrated linearity from 0.03 to 21.52 mg kg^?1. Limits of detection ranged from 6.5 to 86.0 µg kg^?1. The recoveries of spiked samples ranged from 71% to 109%. The procedure was successfully applied in routine inspection analysis.     

Rapid screening of illicit additives in weight loss dietary supplements with desorption corona beam ionisation (DCBI) mass spectrometry

Desorption corona beam ionisation (DCBI), the relatively novel ambient mass spectrometry (MS) technique, was utilised to screen for illicit additives in weight-loss food. The five usually abused chemicals – fenfluramine, N-di-desmethyl sibutramine, N-mono-desmethyl sibutramine, sibutramine and phenolphthalein – were detected with the proposed DCBI-MS method. Fast single-sample and high-throughput analysis was demonstrated. Semi-quantification was accomplished based on peak areas in the ion chromatograms. Four illicit additives were identified and semi-quantified in commercial samples. As there was no tedious sample pre-treatment compared with conventional HPLC methods, high-throughput analysis was achieved with DCBI. The results proved that DCBI-MS is a powerful tool for the rapid screening of illicit additives in weight-loss dietary supplements.     

Determination of phytoestrogens in dietary supplements by LC-MS/MS

Labelling data quantifying the exact content of individual phytoestrogen analytes in dietary supplements are generally poor. As these products are commonly used in the management of menopause symptoms, any clinical benefits would be dependent on the exact dosage of isoflavones received. Well-established extraction procedures and updated isotope dilution mass spectrometry liquid chromatography coupled with tandem mass spectrometry detection (LC-MS/MS) have been used to accurately quantify the concentrations of ten common isoflavones in 35 dietary supplement samples on sale in the UK, Canada and Italy. Concentration-specific ionization suppression is described for biochanin A and formononetin. All supplements contained phytoestrogens. The soya isoflavones (genistein, daidzein, glycitein) were present in all products and the majority also contained the red clover isoflavones (biochanin A, formononetin) and some the Kudzu isoflavones (daidzein, puerarin). The content of total isoflavones per dose ranged from <1 to 53 mg. Trace amounts of coumestrol were found in six products. Other less common analytes, the prenylnaringenins (6-prenylnaringenin, 8-prenylnaringenin, 6,8-diprenylnaringenin) were not found in any of the products. Only 14 of 35 supplements were found to deliver more than or equal to 40 mg day(-1) of aglycone isoflavones, a consensus dose value recognized as delivering therapeutic benefit. Eleven did not match label claims. Six delivered less than 10 mg day (-1) of isoflavones. There has been little improvement in the overall quality of industry labelling in the five years since this was last investigated. Consequently, the public, retailers and healthcare professionals should consider using standardized isoflavone supplements, which are supported by analytical measurements.     

Monitoring of polycyclic aromatic hydrocarbons (PAH) in food supplements containing botanicals and other ingredients on the Dutch market

Food supplements can contain polycyclic aromatic hydrocarbons (PAH). The European Food Safety Authority (EFSA) has defined 16 priority PAH that are both genotoxic and carcinogenic and identified eight priority PAH (PAH8) or four of these (PAH4) as good indicators of the toxicity and occurrence of PAH in food. The current study aimed to determine benzo[a]pyrene and other EFSA priority PAH in different categories of food supplements containing botanicals and other ingredients. From 2003 to 2008, benzo[a]pyrene exceeded the limit of quantification (LOQ) in 553 (44%) of 1258 supplements with a lower-bound mean of 3.37?µg?kg^?1. In 2008 and 2009, benzo[a]pyrene and 12 other EFSA priority PAH were determined in 333 food supplements. Benzo[a]pyrene exceeded the LOQ in 210 (63%) food supplements with a lower-bound mean of 5.26?µg?kg^?1. Lower-bound mean levels for PAH4 and PAH8(-indeno[1,2,3-cd]pyrene) were 33.5 and 40.5?µg?kg^?1, respectively. Supplements containing resveratrol, Ginkgo biloba, St. John's wort and propolis showed relatively high PAH4 levels in 2008 and 2009. Before 2008, supplements with these ingredients and also dong quai, green tea or valerian contained relatively high benzo[a]pyrene levels. On average, PAH4 intake resulting from food supplement use will be at the lower end of the range of contributions of main food groups to PAH4 exposure, although individual food supplements can contribute significantly to PAH4 exposure. Regular control of EFSA indicator PAH levels in food supplements may prove a way forward to reduce further the intake of PAH from food.     

Development and validation of an LC-MS/MS method for the simultaneous analysis of 28 specific narcotic adulterants used in dietary supplements

The purpose of this study was to develop a method to analyse the concentration of multiple illegal narcotics present in dietary supplements. To this end, we established and optimised a procedure using LC-MS/MS simultaneously to analyse 28 narcotic compounds in various forms of dietary supplements, including powders, tablets, liquids and capsules. In addition, candy and cookies that have also had detected cases of adulteration were also analysed. The specificity, linearity, accuracy, precision, limit of detection (LOD), limit of quantitation (LOQ), stability and recovery for these methods were validated accordingly. The LOD and LOQ of the LC-MS/MS ranged from 0.01–50.0 to 0.03–100 ng g^?1, respectively. The linearity of these results was good (r² > 0.99), with intra- and inter-day precision values of 0.2–5.2% and 0.2–4.8%, respectively. Further, the intra- and inter-day accuracies of this method were 97.0–103.4% and 94.6–103.1%, respectively. The stability RSD was less than 7.8%. The mean recovery for this LC-MS/MS procedure was 81.1–117.4%, with an RSD less than 9.8%. Following the validation of our method, we analysed 47 commercially available dietary supplements obtained in Korea. Whilst none of these samples had detectable amounts of the 28 specified narcotic adulterants, our novel LC-MS/MS procedure can be utilised comprehensively and continually to monitor illegal drug adulteration in various forms of dietary supplements.     

Determination of phytoestrogens in dietary supplements by LC-MS/MS.

Labelling data quantifying the exact content of individual phytoestrogen analytes in dietary supplements are generally poor. As these products are commonly used in the management of menopause symptoms, any clinical benefits would be dependent on the exact dosage of isoflavones received. Well-established extraction procedures and updated isotope dilution mass spectrometry liquid chromatography coupled with tandem mass spectrometry detection (LC-MS/MS) have been used to accurately quantify the concentrations of ten common isoflavones in 35 dietary supplement samples on sale in the UK, Canada and Italy. Concentration-specific ionization suppression is described for biochanin A and formononetin. All supplements contained phytoestrogens. The soya isoflavones (genistein, daidzein, glycitein) were present in all products and the majority also contained the red clover isoflavones (biochanin A, formononetin) and some the Kudzu isoflavones (daidzein, puerarin). The content of total isoflavones per dose ranged from <1 to 53 mg. Trace amounts of coumestrol were found in six products. Other less common analytes, the prenylnaringenins (6-prenylnaringenin, 8-prenylnaringenin, 6,8-diprenylnaringenin) were not found in any of the products. Only 14 of 35 supplements were found to deliver more than or equal to 40 mg day(-1) of aglycone isoflavones, a consensus dose value recognized as delivering therapeutic benefit. Eleven did not match label claims. Six delivered less than 10 mg day (-1) of isoflavones. There has been little improvement in the overall quality of industry labelling in the five years since this was last investigated. Consequently, the public, retailers and healthcare professionals should consider using standardized isoflavone supplements, which are supported by analytical measurements.     

Inorganic elemental compositions of commercial multivitamin/mineral dietary supplements: Application of collision/reaction cell inductively coupled-mass spectroscopy

Thirty five different commercially available multivitamin/mineral (MVM) dietary supplements in tablet, capsule, liquid or powder form for children, women, men, young and adult consumption were analysed by collision/reaction cell ICP-MS for their inorganic elemental compositions including Na, Mg, K, Ca, V, Cr, Mn, Fe, Ni, Cu, Zn, As, Se, Cd, Hg, and Pb. Samples were digested with concentrated nitric and hydrochloric acid (8:2) using a closed vessel microwave system. The validity of the applied method was assessed by the analysis of standard reference materials (SRM 3280, SRM 1566b) and of spiked samples. Special emphasis was given to the percentage deviation of calculated daily intake of each analysed element from their corresponding label claim. Additionally, for toxic elements calculated daily intake values are compared with those of the regulatory guideline values (e.g., recommended dietary allowance). The results revealed that all analysed products have calculated daily intake of As, Cd, Pb and Hg concentrations lower than those of the regulatory limits. The percentage differences between the calculated and claimed daily intake values varied moderately (20%) to significantly (>30%) for the potentially toxic elements, especially Cr, Se, Mn, and Zn. Furthermore, it is not uncommon for the same product to have high, as well as low, elemental compositions compared to their corresponding claimed values.     

Determination of multi-class pesticide residue in dietary supplements from grape seed extracts by ultra-high-performance liquid chromatography coupled to triple quadrupole mass spectrometry

A new method was developed and validated for the determination of multi-class pesticide residues in nutraceutical products obtained from grape seed extracts. The extraction procedure was based on QuEChERS methodology using ethyl acetate as solvent and a dispersive solid-phase extraction (dSPE) clean-up stage with C₁₈ was included to minimise matrix effects. Pesticides determination was achieved using ultra-high-performance liquid chromatography coupled to triple quadrupole mass spectrometry (UHPLC-QqQ-MS/MS); total running time was 11 min. Pesticides were quantified using matrix-matched calibration. The developed method was validated in terms of matrix effect, linearity, selectivity, limits of detection and quantification, trueness, repeatability and inter-day precision at three concentration levels (10, 50, 100 µg kg^?1). Suitable recovery values were obtained for 76% of analysed pesticides at the lowest concentration (10 µg kg^?1). For most of the compounds, relative standard deviation values were lower than 20% and 25% for intra- and inter-day precision, respectively. Finally, 106 pesticides were determined, and the method was applied to seven dietary supplements from grape seed extract, obtaining various positive results for piperonyl butoxide, cyromazine and diniconazole at concentrations ranging from 2.0 to 13.4 µg kg^?1.