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Determination of patulin in fruit juice and dried fruit samples by in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry.
J Chromatogr A. 2009 May 01; 1216(18):3746-50.JC

Abstract

A simple and sensitive method for the determination of patulin in fruit juice and dried fruit samples was developed using a fully automated method consisting of in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-mass spectrometry (LC-MS). Patulin was separated within 5 min by high-performance liquid chromatography using a Synergi MAX-RP 80A column and water/acetonitrile (80/20, v/v) as the mobile phase. Electrospray ionization conditions in the negative ion mode were optimized for MS detection of patulin. The pseudo-molecular ion [M-H](-) was used to detect patulin in selected ion monitoring (SIM) mode. The optimum in-tube SPME conditions were 25 draw/eject cycles of 40 microL of sample using a Carboxen 1006 PLOT capillary column as an extraction device. The extracted patulin was readily desorbed from the capillary by passage of the mobile phase, and no carry-over was observed. Using the in-tube SPME LC-MS with SIM method, good linearity of the calibration curve (r=0.9996) was obtained in the concentration range of 0.5-20 ng/mL using (13)C(3)-patulin as an internal standard, and the detection limit (S/N=3) of patulin was 23.5 pg/mL. The in-tube SPME method showed >83-fold higher sensitivity than the direct injection method (10 microL injection volume). The within-day and between-day precision (relative standard deviations) were below 0.8% and 5.0% (n=6), respectively. This method was applied successfully for the analysis of fruit juice and dried fruit samples without interference peaks. The recoveries of patulin spiked into apple juice were >92%, and the relative standard deviations were <4.5%. Patulin was detected at ng/mL levels in various commercial apple juice samples.

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Authors+Show Affiliations

Kataoka H
School of Pharmacy, Shujitsu University, Nishigawara, Okayama 703-8516, Japan. hkataoka@shujitsu.ac.jp
Itano M
No affiliation info available
Ishizaki A
No affiliation info available
Saito K
No affiliation info available

MeSH

BeveragesChromatography, LiquidFruitMass SpectrometryPatulinSensitivity and SpecificitySolid Phase Microextraction

Pub Type(s)

Evaluation Study
Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

19306997

Citation

Kataoka, H, et al. "Determination of Patulin in Fruit Juice and Dried Fruit Samples By In-tube Solid-phase Microextraction Coupled With Liquid Chromatography-mass Spectrometry." Journal of Chromatography. A, vol. 1216, no. 18, 2009, pp. 3746-50.
Kataoka H, Itano M, Ishizaki A, et al. Determination of patulin in fruit juice and dried fruit samples by in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry. J Chromatogr A. 2009;1216(18):3746-50.
Kataoka, H., Itano, M., Ishizaki, A., & Saito, K. (2009). Determination of patulin in fruit juice and dried fruit samples by in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry. Journal of Chromatography. A, 1216(18), 3746-50. https://doi.org/10.1016/j.chroma.2009.03.017
Kataoka H, et al. Determination of Patulin in Fruit Juice and Dried Fruit Samples By In-tube Solid-phase Microextraction Coupled With Liquid Chromatography-mass Spectrometry. J Chromatogr A. 2009 May 1;1216(18):3746-50. PubMed PMID: 19306997.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of patulin in fruit juice and dried fruit samples by in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry. AU - Kataoka,H, AU - Itano,M, AU - Ishizaki,A, AU - Saito,K, Y1 - 2009/03/13/ PY - 2008/12/15/received PY - 2009/02/25/revised PY - 2009/03/06/accepted PY - 2009/3/25/entrez PY - 2009/3/25/pubmed PY - 2009/6/24/medline SP - 3746 EP - 50 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1216 IS - 18 N2 - A simple and sensitive method for the determination of patulin in fruit juice and dried fruit samples was developed using a fully automated method consisting of in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-mass spectrometry (LC-MS). Patulin was separated within 5 min by high-performance liquid chromatography using a Synergi MAX-RP 80A column and water/acetonitrile (80/20, v/v) as the mobile phase. Electrospray ionization conditions in the negative ion mode were optimized for MS detection of patulin. The pseudo-molecular ion [M-H](-) was used to detect patulin in selected ion monitoring (SIM) mode. The optimum in-tube SPME conditions were 25 draw/eject cycles of 40 microL of sample using a Carboxen 1006 PLOT capillary column as an extraction device. The extracted patulin was readily desorbed from the capillary by passage of the mobile phase, and no carry-over was observed. Using the in-tube SPME LC-MS with SIM method, good linearity of the calibration curve (r=0.9996) was obtained in the concentration range of 0.5-20 ng/mL using (13)C(3)-patulin as an internal standard, and the detection limit (S/N=3) of patulin was 23.5 pg/mL. The in-tube SPME method showed >83-fold higher sensitivity than the direct injection method (10 microL injection volume). The within-day and between-day precision (relative standard deviations) were below 0.8% and 5.0% (n=6), respectively. This method was applied successfully for the analysis of fruit juice and dried fruit samples without interference peaks. The recoveries of patulin spiked into apple juice were >92%, and the relative standard deviations were <4.5%. Patulin was detected at ng/mL levels in various commercial apple juice samples. SN - 1873-3778 UR - https://www.unboundmedicine.com/medline/citation/19306997/Determination_of_patulin_in_fruit_juice_and_dried_fruit_samples_by_in_tube_solid_phase_microextraction_coupled_with_liquid_chromatography_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(09)00380-X DB - PRIME DP - Unbound Medicine ER -
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