Detection of Phthalate Esters from Plastic Packaging Materials into Edible Oil by Gas Chromatography-Mass

2013 ◽  
Vol 395-396 ◽  
pp. 355-358 ◽  
Author(s):  
Lin Li ◽  
Qiu Ju Sun ◽  
Shi Gang Xin ◽  
Long Yu ◽  
Zhong Li Jiang
Keyword(s):  
Gas Chromatography ◽  
Edible Oils ◽  
Phthalate Esters ◽  
Correlation Coefficients ◽  
High Sensitivity ◽  
Edible Oil ◽  
Relative Standard ◽  
Two Samples ◽  
Storage Temperatures

A method for the simultaneous determination of 15 kinds of phthalate esters in edible oil by gas chromatography-mass spectrometer (GC-MS) was firstly established. The calibration curves showed good linearity in the range of 0.001~1mg /L and the correlation coefficients (r) were more than 0.999. The limits of quantification were in the range of 0.001~ 2.000 μg/L (S/N = 10). The recovery of three level ranged from 70.50% to 112.00%, at spiked levels of 0.1mg/L, 1.0mg/L and 10mg/L with the relative standard deviations (n = 6) of 0.59% ~ 7.54%. On the basis of the above method, the three edible oils under different storage temperatures were detected and the results showed that DIBP, DBP and DEHP were detected in two samples. This method possesses high sensitivity and low detection limit and can be used for quantitative analysis PAEs in edible oils.

scholarly journals Determination of Six Eugenol Residues in Aquatic Products by Gas Chromatography-Orbitrap Mass Spectrometry

2021 ◽  
Vol 2021 ◽  
pp. 1-9
Author(s):  
Yunxia Huang ◽  
Qiang Li ◽  
Yali Zhang ◽  
Zhijuan Meng ◽  
Xiaoxuan Yuan ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Correlation Coefficients ◽  
Rapid Screening ◽  
Aquatic Products ◽  
Linear Relationships ◽  
Orbitrap Mass Spectrometry ◽  
Relative Standard ◽  
Two Samples

Eugenol compounds are widely used in the circulation and transportation of fresh aquatic products because of their good anesthetic effects. However, some studies have shown that eugenol compounds are potential carcinogens. Therefore, in order to ensure the edible safety of aquatic products, eugenol compounds in aquatic products need to be screened quickly. A method for determination of six eugenol residues in aquatic products was established by multiplug filtration cleanup (m-PFC), combined with gas chromatography-Orbitrap mass spectrometry (Orbitrap GC-MS). Samples were ultrasonically extracted with acetonitrile, and the extracts were frozen at −18°C for 1 h, then purified with the m-PFC column, and detected by Orbitrap GC-MS in full scan mode. The results showed the linear relationships for six eugenols were good in the range of 0.001–0.1 μg/mL, and the correlation coefficients (R2) were above 0.9950. The limits of detection (LODs) were 2–10 μg/kg, and the limits of quantitation (LOQs) were 5–20 μg/kg. The average recoveries at the spiked levels of 5–200 μg/kg were in the range of 76.4%–105.1%, with relative standard deviations (RSDs) of 1.2%–7.5%. Eighty aquatic products were detected by this method, of which only eugenol was detected in 12 samples, and eugenol and isoeugenol were detected in two samples at the same time. The other eugenol compounds were not detected in any sample. The detection rate of positive samples was 17.5%. The method is simple, accurate, and suitable for the rapid screening of eugenol compounds in aquatic products.

scholarly journals Determination of cyanide in bamboo shoots by microdiffusion combined with ion chromatography–pulsed amperometric detection

2018 ◽  
Vol 5 (4) ◽  
pp. 172128 ◽  
Author(s):  
Ming Ding ◽  
Kailiang Wang
Keyword(s):  
Ion Chromatography ◽  
Limit Of Detection ◽  
Correlation Coefficients ◽  
Amperometric Detection ◽  
High Sensitivity ◽  
Practical Method ◽  
Pulsed Amperometric Detection ◽  
Bamboo Shoots ◽  
Relative Standard

A practical method for the determination of cyanide in bamboo shoots has been developed using microdiffusion preparation integrated with ion chromatography–pulsed amperometric detection (IC-PAD). Cyanide was released from bamboo shoots after Conway cell microdiffusion, and then analysed by IC-PAD. In comparison with the previously reported methods, derivatization and ion-pairing agent addition were not required in this proposed microdiffusion combined with IC-PAD method. The microdiffusion parameters were optimized including hydrolysis systems, temperature, time, and so on. Under the optimum conditions, the linear range of the calibration curve for cyanide was 0.2–200.0 µg kg −1 with satisfactory correlation coefficients of 0.9996 and the limit of detection was 0.2 µg kg −1 ( S/N  = 3). The spiked recovery range was from 92.8 to 98.6%. The intra-day and inter-day relative standard deviations of cyanide were 2.7–14.9% and 3.0–18.3%, respectively. This method was proved to be convenient in operation with high sensitivity, precision and accuracy, and was successfully applied in the determination of cyanide in bamboo shoot samples.

Determination of Phthalate Esters in Wastewater by Single-Drop Microextraction Coupled to Capillary Gas Chromatography

2013 ◽  
Vol 295-298 ◽  
pp. 483-486 ◽  
Author(s):  
Jian Qi Sun
Keyword(s):  
Gas Chromatography ◽  
Capillary Gas Chromatography ◽  
Phthalate Esters ◽  
Wastewater Sample ◽  
Single Drop ◽  
Flame Ionization ◽  
Single Drop Microextraction ◽  
Relative Standard ◽  
Wastewater Samples

Single-drop microextraction (SDME) coupled to capillary gas chromatography (GC) was established for the determination of four phthalate esters in wastewater, including dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-octyl phthalate (DnOP) and butyl benzyl phthalate (BBP). The SDME parameters such as extractants, extracting time，stirring rate and immerging depth of needle point were studyed and optimized. The abovementioned phthalate esters were quantified by external standardization method using GC coupled with a flame ionization detector (FID). The linear regression calibration curves, detection limits (S/N=3) and the linear ranges of the method for determining each phthalate were determined, respectively. The concentrations of components abovementioned in a real wastewater sample, the average of the recoveries obtained in the spiked wastewater samples and the corresponding relative standard deviations were determined, respectively. The results showed the proposed method several attributes, friendly enviroment, economic and highly efficient pretreatment, less time, simplicity, sensitivity, accuracy and wide linear range and so on.

scholarly journals SIMULTANEOUS DETERMINATION OF BENZYDAMINE HYDROCHLORIDE, METHYLPARABEN AND PEPPERMINT OIL IN A SPRAY DOSAGE FORM BY GAS CHROMATOGRAPHY

2019 ◽  
pp. 147-153
Author(s):  
VASYL A. CHORNYI ◽  
VICTORIYA A. GEORGIYANTS ◽  
SVITLANA N. GUREEVA ◽  
OLGA V. CHORNA
Keyword(s):  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Dosage Form ◽  
Analytical Procedure ◽  
Correlation Coefficients ◽  
Peppermint Oil ◽  
Chromatography Method ◽  
Relative Standard ◽  
Validation Parameters

Objective: To develop and validate an analytical procedure for simultaneous determination of benzydamine hydrochloride, methylparaben and peppermint oil in a spray dosage form by gas chromatography method (GC). Methods: The analytical method was conducted on Agilent 7890 gas chromatograph, equipped with HP-5 capillary column with helium as a mobile phase, split/splitless injector and flame ionization detector and an auto injector. Validation parameters, such as selectivity, linearity, precision, accuracy and, robustness were estimated. Results: A method for simultaneous determination of benzydamine hydrochloride, methylparaben and peppermint oil in a spray dosage form by GC was developed. The retention time of menthol (marker substance of peppermint oil) methylparaben and benzydamine hydrochloride, was 5.0, 9.2, and 19.4 respectively. Relative standard deviation (RSD)% for precision was 0.24, 0.13 and 0.12 respectively. The linearity of the method for given analytes was estimated in a concentration range of 80-120% to a nominal concentration with the respective correlation coefficients of more than 0.999. Accuracy of the method was within 98-102% for all analytes. Conclusion: The developed analytical procedure meets the acceptance criteria of validation parameters and can be used in quality control laboratories for determination of benzydamine hydrochloride, methylparaben and peppermint oil in a spray dosage form.

Simultaneous Determination of Benefin and Trifluralin in Pesticide Formulations by Gas Chromatography

1990 ◽  
Vol 73 (6) ◽  
pp. 981-982
Author(s):  
Timothy M Fitzpatrick ◽  
Connie C Gehrig
Keyword(s):  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Correlation Coefficients ◽  
Flame Ionization Detection ◽  
Least Squares Regression ◽  
Flame Ionization ◽  
Pesticide Formulations ◽  
Relative Standard ◽  
Peak Areas

Abstract Formulations containing benefin and trifluralin are extracted In hexane and determined using direct splltless capillary gas chromatography with flame Ionization detection. Resolution of the Isomers Is approximately 0.8 for run times of 20 mln. Least-squares regression of peak areas against concentrations for the simultaneous determination of the 2 Isomers produced correlation coefficients of 0.9999 and 0.9990 for benefin and trifluralin, respectively. These compare favorably with the linearities of each Isomer Individually. Quadruplicate analyses of 4 ground fertilizer formulations produced an average relative standard deviation of 1.98%. Recoveries were erratic for granular fertilizer formulations but were 105 ± 3.6% for a liquid trifluralin formulation spiked with both trifluralin and benefin.

scholarly journals Determination of Five Phthalate Esters and Bisphenol A in Fruit Juice by Packed-nanofiber Solid Phase Extraction Coupled with Gas Chromatography

2019 ◽  
Vol 8 (1) ◽  
pp. 50-54 ◽  
Author(s):  
Zigang Tang ◽  
Tao Kang ◽  
Xuejun Kang
Keyword(s):  
Gas Chromatography ◽  
Bisphenol A ◽  
Solid Phase Extraction ◽  
Fruit Juice ◽  
Solid Phase ◽  
Phthalate Esters ◽  
Phase Extraction ◽  
Relative Standard ◽  
Juice Sample

Packed-nanofiber solid phase extraction   (PFSPE) combined with gas chromatography-flame ionization detector (GC-FID) was developed for the simultaneous determination of five phthalate esters (PAEs) and bisphenol A (BPA) in fruit juice. The PAEs and BPA was concentrated by PFSPE using polystyrene- pyridine (PS-PD) nanofibers as the sorbent, followed determined by GC-FID. Under this modified procedure, satisfied recoveries in fruit juice sample ranging from 81.9% to 109.6% were obtained. And relative standard deviation values (RSD) were ranged from 1.9 % to 9.8% in orange juice sample. The limits of detection (LOD) and the limits of quantification (LOQ) of five PAEs and BPA were ranged from 0.02 μg/mL to 0.30 μg/mL and 0.06 μg/L to 1.10 μg/L, respectively. This established method was successfully applied to detect real fruit juice samples, which were collected in local supermarket. These results demonstrated the applicability of the established PFSPE-based extraction coupled with gas chromatography method for determination of PAEs and BPA in fruit juice products.

Atomic absorption determination of Hg (II), Cd (II), and As (III) in natural and waste water after preliminary group preconcentration

2019 ◽  
Vol 85 (2) ◽  
pp. 12-16
Author(s):  
I. V. Saunina ◽  
E. N. Gribanov ◽  
E. R. Oskotskaya
Keyword(s):  
Waste Water ◽  
Atomic Absorption ◽  
High Sensitivity ◽  
Distribution Coefficients ◽  
Neutral Medium ◽  
Atomic Absorption Determination ◽  
Absorption Determination ◽  
Relative Standard ◽  
Preliminary Group

The sorption of Hg (II), Cd (II), and As (III) by natural aluminosilicate is studied. It is shown that the mineral absorbs those toxicants in a rather wide pH range, quantitative extraction of analytes being achieved in a neutral or close to neutral medium (pH values range within 7.0 - 8.0; 6.3 - 7.5; 7.4 - 8.5 for Hg (II), As (III), and Cd (II), respectively). The effect of the time of phase contact on the degree of extraction of elements is shown. The sorption capacity of the mineral in optimal conditions of the medium acidity (0.06 mmol/g for mercury, 0.31 mmol/g for cadmium, and 0.52 mmol/g for arsenic) is determined. The distribution coefficients attain values of aboutnX 103-nX 104. A new combined method for determination of Hg (II), Cd (II), and As (III) in natural and waste water is developed and tested. The method consists in a preliminary group sorption concentration of the analytes by aluminosilicate, desorption of the analytes from the surface of the mineral and their subsequent atomic absorption determination. The correctness of the method is verified in analysis of spiked samples. The method is easy to use and exhibits high sensitivity, reproducibility and accuracy of analyte determination. The relative standard deviation does not exceed 0.13. Economic availability and possibility of using domestic sorption materials are the important advantages of the proposed procedure which can be used in the practice of laboratories monitoring the quality and safety of environmental objects.

Determination of Selected Phthalates in Some Commercial Cosmetic Products by HPLC-UV

2020 ◽  
Vol 23 (10) ◽  
pp. 1010-1022
Author(s):  
Emrah Dural
Keyword(s):  
High Performance ◽  
Phthalate Esters ◽  
High Sensitivity ◽  
Hplc Method ◽  
Cosmetic Products ◽  
Limit Of Quantification ◽  
Nail Polish ◽  
Accuracy And Precision ◽  
Butyl Phthalate

Aim and scope: Due to the serious toxicological risks and their widespread use, quantitative determination of phthalates in cosmetic products have importance for public health. The aim of this study was to develop a validated simple, rapid and reliable high-performance liquid chromatography (HPLC) method for the determination of phthalates which are; dimethyl phthalate (DMP), diethyl phthalate (DEP), benzyl butyl phthalate (BBP), di-n-butyl phthalate (DBP), di(2- ethylhexyl) phthalate (DEHP), in cosmetic products and to investigate these phthalate (PHT) levels in 48 cosmetic products marketing in Sivas, Turkey. Materials and Methods: Separation was achieved by a reverse-phase ACE-5 C18 column (4.6 x 250 mm, 5.0 μm). As the mobile phase, 5 mM KH2PO4 and acetonitrile were used gradiently at 1.5 ml min-1. All PHT esters were detected at 230 nm and the run time was taking 21 minutes. Results: This method showed the high sensitivity value the limit of quantification (LOQ) values for which are below 0.64 μg mL-1 of all phthalates. Method linearity was ≥0.999 (r2). Accuracy and precision values of all phthalates were calculated between (-6.5) and 6.6 (RE%) and ≤6.2 (RSD%), respectively. Average recovery was between 94.8% and 99.6%. Forty-eight samples used for both babies and adults were successfully analyzed by the developed method. Results have shown that, DMP (340.7 μg mL-1 ±323.7), DEP (1852.1 μg mL-1 ± 2192.0), and DBP (691.3 μg mL-1 ± 1378.5) were used highly in nail polish, fragrance and cream products, respectively. Conclusion: Phthalate esters, which are mostly detected in the content of fragrance, cream and nail polish products and our research in general, are DEP (1852.1 μg mL-1 ± 2192.0), DBP (691.3 μg mL-1 ± 1378.5) and DMP (340.7 μg mL-1 ±323.7), respectively. Phthalates were found in the content of all 48 cosmetic products examined, and the most detected phthalates in general average were DEP (581.7 μg mL-1 + 1405.2) with a rate of 79.2%. The unexpectedly high phthalate content in the examined cosmetic products revealed a great risk of these products on human health. The developed method is a simple, sensitive, reliable and economical alternative for the determination of phthalates in the content of cosmetic products, it can be used to identify phthalate esters in different products after some modifications.

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