scholarly journals Determination of Patulin in Apple Juice by Liquid Chromatography

2006 ◽  
Vol 89 (1) ◽  
pp. 139-143 ◽  
Author(s):  
Maria Helena Iha ◽  
Myrna Sabino

Abstract A method was developed and validated in-house for the determination of patulin (PAT), a toxic mold metabolite, in apple juice. The sample was extracted with ethyl acetatehexane and analyzed by liquid chromatography equipped with a C18 column and diode array detector. The mobile phase used for the quantification was waterethanol, at a flow rate of 0.5 mL/min. The method showed a mean recovery of 84.8%, the relative standard deviation obtained in the precision study was <7.7%, the quantification and detection limits were 7 and 3 μg/L, respectively, and the linear range for PAT in apple juice was 2.6650 μg/L. The ruggedness was evaluated by an intralaboratory experiment, in which 5 factors were studied, and only one was found to influence the observed results. The developed method is fast, practical, and simple; the solvents (except hexane) and reagents used were nontoxic. The results of the validation confirmed the efficiency of the method, which is sensitive enough to be used in studies required to quantify PAT in apple juice.

Author(s):  
Thu Dam Thi ◽  
Kieu Anh Nguyen Thi ◽  
Thanh Phuong Nguyen Thi ◽  
Hong Hanh Nguyen Thi ◽  
Dat Nguyen Thanh ◽  
...  

A method using solid phase extraction (SPE) and high performance liquid chromatography with diode array detector (HPLC-DAD) has been optimized for the simultaneous determination of notoginsenoside R1 and three ginsenosides Rg1, Re, Rb1 in solid, oil, and liquid dietary supplements. The substances were separated by an InertSustain C18 column (250 mm × 4.6 mm i.d.; particle size 5 μm) with a gradient program composed of acetonitrile and water. Linearities were in the range of 4.0 - 400 μg/mL with the coefficients of determination were more than 0.999. The limits of detection and limits of quantitation were 2.13 - 6.89 μg/g and 7.11 - 22.98 μg/g, respectively. The recovery values of the compounds were in the range of 87.2 - 103.5%. The precision study showed the intra-day relative standard deviation (RSD) of 1.41 - 2.91%, and inter-day RSD of 1.87 - 4.85%, which meet the AOAC International requirements. The method was applied to determine the content of notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, and ginsenoside Rb1 in 20 dietary supplement samples containing Ginseng and Pseudoginseng.


2013 ◽  
Vol 694-697 ◽  
pp. 1047-1050
Author(s):  
Hong Jun Wang ◽  
Tie Zhong Zhou ◽  
Hong Jiang ◽  
Dan Yao ◽  
Tie Liang Wang ◽  
...  

Bangduling (BDL) oral liquid, which is a new research and development herbal preparation, comprises four traditional Chinese medicines (TCM): Radix Scutellariae, Cortex Phellodendri Chinensis, Folium Isatidis, and Radix et Rhizoma Rhei. A simple, reliable and reproducible method, based on a high performance liquid chromatography-diode array detector (HPLC-DAD) method, for establishing fingerprint of complex herbal medicine BDL oral liquid was described firstly. In order to develop and validate this HPLC-DAD method, Kromasil C18 column (S-5μm, 4.6 mm × 250 mm) was used with gradient mobile phase at the column temperature of 30°C. The mobile phase was consisted of methanol and water containing 0.1% phosphoric acid. UV wavelength was set at 254 nm. Ten batches of BDL preparations were used to establish the HPLC fingerprint. In addition, the contents of baicalin in the preparations were also determined. Validation of the analytic method was evaluated by stability, precision and repeatability test. Calibration curve for baicalin showed good linearity with R2 = 0.9992. The relative standard deviations (RSDs) value of the relative retention time and peak area in the stability, precision and repeatability test, were less than 1% and 5%, respectively. The similarity of 10 batches of BDL oral liquid was more than 0.958, which showed the preparations from different batch productions were consistent. This established determination method could be efficient to the quality control of BDL oral liquid.


2012 ◽  
Vol 27 (4) ◽  
pp. 321-329 ◽  
Author(s):  
Sanja Lazic ◽  
Dragana Sunjka ◽  
Nada Grahovac ◽  
Valéria Guzsvány ◽  
Ferenc Bagi ◽  
...  

A rapid and simple method for simultaneous determination of acetamiprid and its metabolite 6-chloronicotinic acid in sweet cherry samples has been developed. This residue analysis method is based on the reversed phase separation on C18 column with gradient elution. Analytes? determination and quantification were performed by high performance liquid chromatography (HPLC) with diode-array detector and chromatograms were extracted at 230 nm. Extraction efficiency experiments demonstrated the ability of this method to extract neonicotinoids from sweet cherry samples. These insecticides were extracted with a mixture of acetonitril/0.1N ammonium-chloride (8/2, v/v). The average recoveries of acetamiprid and 6-chlornicotinic acid from sweet cherry samples were in the range of 95-101% and 73-83%, respectively, with the associated relative standard deviations (RSDs) <5%. Expanded measurement uncertainties for the analyzed compounds were 2.7 and 3.01%. The limit of quantification (LOQ) was 10 ?g/kg and 30 ?g/kg for acetamiprid and 6-chloronicotinic acid, respectively. Thus, the developed HPLC/DAD method can be considered a useful tool for sensitive and rapid determination of acetamiprid and 6-chloronicotinic acid. Hence, the method may find further application in the analysis of real sweet cherry samples contaminated with these insecticides at a ppb level.


2016 ◽  
Vol 8 (26) ◽  
pp. 5212-5217 ◽  
Author(s):  
M. C. A. Marcelo ◽  
T. R. Fiorentin ◽  
K. C. Mariotti ◽  
R. S. Ortiz ◽  
R. P. Limberger ◽  
...  

A liquid chromatography with a diode array detector (LC-DAD) method was developed through Doehlert optimization for analysis of cocaine seized in the state of Rio Grande do Sul, Brazil.


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