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| Determination of 7 Antioxidants in Rubber Seal Gaskets for Food Contact by Liquid Chromatography－Tandem Mass Spectrometry |
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| DOI： |
| KeyWord:liquid chromatography－tandem mass spectrometry rubber seal gasket for food contact antioxidant microwave extraction |
| Author | Institution |
| CHENG Chang，LU Li-xin，PAN Liao，LU Li-jing，CHEN Xi |
1. Department of Packaging Engineering， School of Mechanical Engineering， Jiangnan University， Wuxi ， China; 2. Jiangsu Key Laboratory of Advanced Food Manufacturing Equipment Technology， Wuxi ， China |
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| Abstract: |
| A method was developed for the determination of residues of 7 antioxidants， i.e. antioxidant ZKF， antioxidant 259， antioxidant 1035， antioxidant 425， antioxidant 2246， antioxidant 1520 and antioxidant 565 in rubber seal gaskets for food contact by liquid chromatography－tandem mass spectrometry. By optimizing the chromatographic column， elution procedure and mass spectrometry conditions， the optimal detection conditions were determined. The rubber powder sample was obtained by freezing and grinding the rubber sample with a freezing grinding instrument. After comparing the recoveries of three kinds of filter membranes and high-speed centrifugation， the high-speed centrifugation method was adopted to pretreat the extract. In addition， three extraction methods including ultrasonic， reflux and microwave， and two extraction solvents including methanol and acetone were used to extract the antioxidants from the positive rubber powder samples to obtain the extraction solution. Microwave extraction with methanol was determined as the optimal pretreatment method with the extraction recovery and extraction efficiency as the evaluation indexes. The rubber powder samples（g） and methanol（mL） were mixed by the ratio of 1∶20， then extracted at 50 ℃ for 15 minutes under microwave condition. After high-speed centrifugation treatment， the extracted liquid samples were detected by liquid chromatography－tandem mass spectrometry. The separation was performed on an Acquity UPLC BEH C18（100 mm × 2.1 mm， 1.7 μm） column by gradient elution with acetonitrile－ammonium acetate aqueous solution（5 mmol/L） as the mobile phase， and the determination was carried out in positive and negative ion modes. Results showed that the limits of detection（LOD）， limits of quantitation（LOQ）， method limits of detection（MLOD） and method limits of quantitation（MLOQ） for the 7 antioxidants were in the ranges of 0.003－0.083 μg/L， 0.01－0.25 μg/L， 0.005－0.125 mg/kg and 0.02－0.40 mg/kg， respectively. There were good linear relationships for the 7 antioxidants in the mass concentration range of 0.01－0.5 mg/L， with their correlation coefficients（r2） all greater than 0.999. The average recoveries ranged from 73.1% to 120% with relative standard deviations（RSD， n=6） of 0.70%－9.3%， which indicated that the developed method was stable and accurate. Finally， 8 kinds of commercial food contact rubber gasket samples were detected by this method. It was found that antioxidant 259， antioxidant 425， antioxidant 1520 and antioxidant 2246 were detected in the commercial samples， while the others were undetected. This method could be used to detect 7 kinds of antioxidants simultaneously within 15 min， with a fast detection speed and a low detection limit， which could meet the needs for detection of antioxidants in food contact rubber materials and products. |
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