Sildenafil and analogous phosphodiesterase type 5 (PDE-5) inhibitors in herbal food supplements sampled on the Dutch market.

Herbal food supplements, claiming to enhance sexual potency, may contain deliberately added active pharmacological ingredients (APIs) that can be used for the treatment of erectile dysfunction (ED). The aim of this study was to determine whether herbal food supplements on the Dutch market indeed contain APIs that inhibit phosphodiesterase type 5 (PDE-5) inhibitors, such as sildenafil and analogous PDE-5 inhibitors. Herbal food supplements intended to enhance sexual potency (n = 71), and two soft drinks, were sampled from 2003 up to and including 2012. In 23 herbal supplements, nine different PDE-5 inhibitors were identified; in a few cases (n = 3), more than one inhibitor was indentified. The presence of these APIs was however not stated on the label. The concentrations of PDE-5 inhibitors per dose unit were analysed. Furthermore, the potential pharmacologically active properties of the detected PDE-5 inhibitors were estimated by using data from the scientific and patent literature regarding (1) in vitro PDE-5 activity, (2) reported effective doses of registered drugs with PDE-5 inhibitor activity and (3) similarity to other structural analogues. It was concluded that 18 of the 23 herbal food supplements, when used as recommended, would have significant pharmacological effects due to added APIs. Adequate use of existing regulation and control measures seems necessary to protect consumers against the adverse effects of these products.

Levels of lead, arsenic, mercury and cadmium in clays for oral use on the Dutch market and estimation of associated risks.

Pregnant women in Africa, Asia and Suriname, and some immigrants in Western societies, traditionally consume clay products known by a variety of names such as mabele, calabash chalk, sikor and pimba. Furthermore, clay is used for health purposes in Western societies. Because certain clays can contain high levels of metals and metalloids, the aim of this study was to determine lead, arsenic, mercury and cadmium in clay products for oral use available on the Dutch market. Traditional clays originating from Africa (n = 10) and Suriname (n = 26), and health clays (n = 27) were sampled from 2004 up to and including 2012. Total metal and metalloid contents were measured by ICP-MS and showed maximum levels of lead, arsenic, mercury and cadmium of 99.7, 45.1, 2.2 and 0.75 mg kg⁻¹, respectively. In the absence of maximum limits for these type of clays, the potential exposure was estimated from the determined concentration, the estimated daily use level of the clays, and the estimated bioaccessibility of the different metals and arsenic. The intake estimates were compared with existing health-based guidance values. For lead, the use of 34 of the 36 traditional clays and two of the 27 health clays would result in intake levels exceeding the toxicological limit by up to 20-fold. Use of 15 of the 35 traditional clays and 11 of the 27 health clays would result in intake levels exceeding the toxicological limit for inorganic arsenic by up to 19-fold. Although limited bioaccessibility from the clay may limit the exposure and exceedance of the health-based guidance values, it was concluded that lead and arsenic intakes from some clay products could be of concern also because of their use by pregnant women and the potential developmental toxicity. As a result the use of these products, especially by pregnant women, should be discouraged.

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.

Monitoring of mercury, arsenic, and lead in traditional Asian herbal preparations on the Dutch market and estimation of associated risks.

Traditional herbal preparations used in Ayurveda, traditional Chinese medicine, traditional Tibetan medicine, and other Asian traditional medicine systems may contain significant amounts of mercury, arsenic or lead. Though deliberately incorporated in Asian traditional herbal preparations for therapeutic purposes, these constituents have caused intoxications worldwide. The aim of this study was therefore to determine mercury, arsenic, and lead levels in Asian traditional herbal preparations on the Dutch market. A total of 292 traditional herbal preparations used in Ayurveda, traditional Chinese medicine, and traditional Tibetan medicine were sampled between 2004 and 2007. Samples were mostly multi-ingredient traditional herbal preparations containing herbs and minerals. The labeling of less than 20% of the traditional herbal preparations suggested the presence of mercury, arsenic or lead. These elements were shown by inductively coupled mass spectrometry (ICP-MS) in 186 (64%) of 292 traditional herbal preparations. Estimated weekly mercury, arsenic, and lead intake levels were calculated for each traditional herbal preparation from the analytically determined concentrations and the recommended dose. A total of 59 traditional herbal preparations (20%) were likely to result in intakes of these elements significantly exceeding safety limits. Of these 59 traditional herbal preparations, intake estimates for 50 traditional herbal preparations significantly exceeded the safety limit for mercury (range = 1.4-1747 mg week(-1)); intake estimates for 26 traditional herbal preparations significantly exceeded the safety limit for arsenic (range = 0.53-427 mg week(-1)) and intake estimates for eight traditional herbal preparations were significantly above the safety limit for lead (range = 2.6-192 mg week(-1)). It is concluded that the mercury, arsenic, and lead contents of traditional herbal preparations used in Ayurveda, traditional Chinese medicine, and traditional Tibetan medicine remain a cause for concern and require strict control.

Determination of the level of benzo[a]pyrene in fatty foods and food supplements.

A routine method was developed for the quantification of benzo[a]pyrene (BaP) in edible oils and food supplements. BaP is often taken as an indicator of the presence of polycyclic aromatic hydrocarbons. The method consists of on-line liquid chromatography clean-up followed by injection to an HPLC system with fluorescence detection. The method has good performance characteristics and gave good results in proficiency tests. From 2002 to 2004, about 1350 samples of oils and food supplements were analysed using this method to test the level of BaP. About 20% of the edible oils contained more than 1.2 microg kg-1 BaP (which is the limit applied by the Dutch Food and Consumer Product Safety Authority until 1 April 2005, and includes measurement uncertainty). In the case of food supplements, more then 30% contained too high levels of BaP, ranging from 1.2 to 135 microg kg-1.

Determination of selected phytochemicals by reversed-phase high-performance liquid chromatography combined with ultraviolet and mass spectrometric detection.

A robust, routinely manageable and sensitive RP-HPLC method combined with UV (270 nm) and ESI-MS detection was established for the determination of abundant pertinent phenolic compounds (phytochemicals) from various biological matrices. Phytochemicals were extracted by aqueous methanol (80%), extracts were analysed without further purification. Baseline separation was achieved within 30 min for 19 phytochemicals and excellent sensitivity (6-42 pmol at S/N = 3) was obtained. The identity of the phytochemicals was confirmed with standard compounds and with LC-MS. The repeatabilities for the majority of the phytochemicals ranged between 3% and 6%. The practicability of the method was shown in complex biological matrices by analysing onion and soybean extracts. This generally applicable technique may serve as a valuable tool for a rapid screening and a specific measurement of phytochemicals in food extracts and biological fluids and serve as analytical instrument for future biochemical and physiological studies.