LC-ESI-MS/MS identification of oleuropein as marker of Olea europaea L., leaves used as a bulking agent in ground oregano and sage

The identification of the secoiridoid oleuropein by LC-ESI-MS/MS (negative) is demonstrated for the quality control directed toward confirmation of the presence of Olea europaea L. leaves used as bulking agent in ground oregano and sage. The described operating conditions are useful for the simple qualitative identification of this marker of O. europaea L. leaves. No tolerance limits are defined for the presence of the above mentioned extraneous vegetable material in ground oregano and sage, the herbs which have been identified in various cases as adulterated with O. europaea L. leaves. Despite the importance of quality control of aromatic herbs, only a limited number of papers have been published on the identification of phenolic compounds as markers of adulteration. The proposed method is simple and suitable for rapid routine analysis

Identification of perflurooctanoic acid release from commercial coated cooking pans by liquid chromatography coupled to electrospray ionization tandem mass spectrometry

Salts of perfluorooctanoic acid (PFOA) can be used in the manufacture of fluoropolymers employed for coating pans; moreover, PFOA can be formed as a byproduct of thermolysis of the aforesaid fluoropolymers. This study was carried out to evaluate PFOA migration into food cooked in fluoropolymer-coated pans. The pans were purchased from a local retailer and subjected to cooking conditions. Used oil was extracted with a methanol/water solution and analyzed by liquid chromatography tandem mass spectrometry (LC/MS/MS). We found that PFOA can enter cooked food during a container's first phases of use, not only in containers already abused by kitchen tools or otherwise scratched

Determination of furan by headspace solid-phase microextraction\u2013 gas chromatography\u2013mass spectrometry in balsamic vinegars of Modena (Italy)

An isotope dilution method for quantification of furan by internal standardization was adopted, using head space solid phase microextraction (HS-SPME) technique, to evaluate various samples of \u2018\u2018aceto balsamico di Modena\u2019\u2019 (ABM), in order to verify if this seasoning may contribute to the intake of furans in the human diet. Matrix-matched calibration curves were adopted, and furan levels in the majority of the samples purchased on the Italian market ranged between 4 and 26 ng/g. Considering that furan levels in ABM derive from the heat-concentrated must of grapes and from the additive caramel E 150d often used in the production technology, the level of furan in the concentratedmust appears, in some samples, not to be the only important factor affecting the risk assessment of furan linked to the use of ABM

Headspace-SPME Analysis of Volatiles from Quince Whole Fruits

Solid-phase microextraction (SPME) combined with GC and GC/MS was used for analysis of the volatile compounds of quince (Cydonia oblonga Mill.). The whole fruits, representing two different ripening stages, were stored and analyzed one day after collection. More than 40 volatile compounds were identified. The relative percentage of acetates, with exception of (Z)-3-hexenyl acetate, increased in a parallel way with ripeness. Of the esters of higher organic acids, ethyl hexanoate and ethyl octanoate were present in the greatest quantity. Ethyl octanoate, which was present in the highest quantity, showed the highest increase with ripeness (from 6\u20138% to 15\u201318%), while ethyl hexanoate increased 3% to >4%. In contrast, the relative percentages of two sesquiterpenes, a-bergamotene and a-farnesene, clearly decreased with ripeness

Preliminary data on volatile composition of olive fruits of cv. "Simona" and possible relationship to resistance to fly oviposition

By characterizing the volatile compounds of the olive cultivar \u201cSimona\u201d from southern Italy (Apulia region), we identified a way to analyze characteristics possibly linked to this olive\u2019s well-known resistance to fly oviposition. The pool of volatile compounds in the unripe and ripe fruits was identified, and even if the relative amounts of these compounds tended to vary with ripening, the fly repellent action appeared to be related to the sesquiterpenes such as alpha-copaene, cycloisosativene, alpha-muurolene, beta-cubebene and hydrocarbons such as (E)-2-dodecene, undecane, tridecane, and 3-methyl undecane. In agreement with the concept that the collective pool of volatile substances can enhance olfactory pleasure/repulsion more than would the effects of a single compound, the pool of volatile compounds identified in this paper may be among the possible characteristic mixtures with repellent action against Bactrocera oleae. The selection of volatile compounds made by the cuticle and responsible of the headspace quality surrounding the whole olive fruit is also demonstrated to be markedly different from the headspace volatile compounds produced by the extracted oil

Determination of gamma-butyrolactone (GBL) in foods by SBSE-TD/GC/MS

4-hydroxybutyric acid lactone, or gamma-butyrolactone (GBL), is a molecule included in the FEMA (Flavor Extract Manufacturers Association) list of flavouring substances (No. 3291) and used as natural-identical substance in flavouring formulation. Recently, the use of GBL has been subjected to restrictions by FDA because, together with the conversion derivative GHB (gamma-hydroxybutyric acid), it has been recognized and classified as psychotropic. In 1999 the Italian law included GBL in the list of psychotropic substances and more recently in the Table of substances inducing psychic and physical addiction. However, GBL has been detected in several natural products. Under a toxicological point of view the difference between natural and natural-identical GBL in food is not relevant. In any case, the evaluation of the total content of GBL in many foods contributes to evaluate the consumption ratio and the aim of this paper is to evidence the possibility of detecting GBL with a high sensitivity method also in complex matrices with analytical procedure characterized by high recovery. This paper proposes a new, simplified, sensitive and selective method (SBSE-TD/GC/MS) useful to detect and quantify the GBL in foods. The work shows, as an application of this method, the detection of this molecule in the very complex matrix of a confectionery product on the international market. The reliability of the method was verified by recovery and repeatability tests. Recovery average values result between 85\u201392% (CV%=8.2\u20135.3) for the concentration range 1\u201310mg/l and between 92\u201395% (CV%=6.5\u20134.2) for the concentration range 10\u201325mg/l

Determination of capsaicinoids from dried pepper fruits by Fast-Gas Chromatography

The present paper describes the application of Fast-gas chromatography (GC) to quantify the capsaicinoid content in dried pepper fruit with the aim to calculate the Scoville heat values (SHVs) for routine quality control. Fast-GC was used to analyse various samples of dried pepper fruits with a wide distribution of SHVs. The calibration curves demonstrated a polynomial model in the range of 3.0-195.0 \u3bcg mL-1 for capsaicin and 2.6-105.0 \u3bcg mL-1 for dihydrocapsaicin and nordihydrocapsaicin, with correlation coefficients of 0.996 and 0.997, respectively. The data showed an intraday relative standard deviation (RSD) <5% and an interday relative repeatability standard deviation (RSDr) <6%

Determination of ethylene chlorhydrin as marker of spices fumigation with ethylene oxide

Ethylene oxide (EO) is a gas used to sterilize spices, drugs, packaging materials, medical devices, polyester fibers, plastics and synthetic rubber. When the aeration step foreseen for spices is not properly carried out, residues of EO and its deriv. ethylene chlorohydrin (ECH), produced by reaction with chlorine ions always present in the matrix, can be found in these products. In this way, the reactivity of EO with chlorides in spices provides a suitable marker to confirm the use of EO for fumigation. The ECH derived from spontaneous transformation during the storage and forcibly obtained during the first step of the extn. can be evaluated in spices by a simple GC/MS anal. method, without derivatization. It has been proven that the EO mol. is carcinogenic for humans; it has been classified as a category 1 carcinogen by the International Agency for Research on Cancer (IARC): ECH, as EO, is a mutagenic substance. This paper shows the results concerning 25 pepper samples purchased on the Italian market. The limit of detection for ECH was assumed to be 20 ?g/kg (LOD) and was calcd. by spiking a matrix pepper that had not been treated with EO. The limit of quantitation was assumed to be 100 ?g/kg (LOQ), i.e. 5 times LOD. The reliability of the method was verified by recovery and repeatability tests. Recovery av. values are 60-70% (CV% = 9.6-5.5) for the concn. range 100-500 ?g/kg. Only 56% of pepper samples analyzed did not contain ECH at detectable levels, and only 24% of pepper samples contained ECH at levels lower than LOQ. Three samples had a content ranging between 0.2 and 3.3 mg/kg and two samples showed a content of ECH higher than 5 mg/kg

Fast Determination of Sudan I by HPLC/APCI-MS in Hot Chilli, Spices, and Oven-Baked Foods

The Commission Decision of EC dated 20 June 2003, on emergency measures concerning hot chilli and hot chilli products coming into any EC member state, required that the consignments of such products should be accompanied by an analytical report showing that they are free of artificial dye Sudan I. The opportunity to set a confirmatory method is evident, and the paper proposes a HPLC/APCI-MS method useful for identification and quantitation of Sudan I, also at very low levels in hot chilli, other spices, and oven-baked foods. Validation data are reported

Identification of Diisobutyl Phthalate (DIBP) Suspected as Possible Contaminant in Recycled Cellulose for Take-away Pizza Boxes

Italian law specifically requires the use of virgin, rather than recycled, cellulose in the production of pizza boxes. We investigated the frequent failure to comply with this law: the identification and determination of phthalates, which have widespread use, contribute to the quality control of various food packaging materials. Diisobutyl phthalate (DIBP) has similar structural and application properties to di-n-butyl-phthlate (DBP), and it is used as a substitute for DBP. We standardized an analytical method that allows the calculation of an \u2018exposure index\u2019 (EI) for DIBP in take-away pizza boxes. The technique, which relies on Solid-Phase Micro Extraction/Gas Chromatography/Mass Spectrometry (SPME/GC/MS), allows the definition of a large range of DIBP content in the headspace within various take-away pizza boxes. Data concerning pizza boxes purchased in 16 restaurants in 2006 were reported, and the \u2018EIs\u2019 were estimated to range between 6 and 72 microg