LC-MS/MS를 이용한 소시지 중 보존료 동시분석
Simultaneous determination of preservatives in sausages using liquid chromatography with electrospray ionization tandem mass spectrometry
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초록
A simultaneous determination method was developed for nine preservatives (benzoic acid, sorbic acid, dehydroacetic acid, methyl-, ethyl-, isopropyl-, propyl-, isobutyl- and butyl-parabens) in sausage by liq-uid chromatography with electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS). Each pa-rameter was established by multiple reaction monitoring in negative mode. Separation was achieved on a phenyl-hexyl (2.5 m, 2.1×150 mm, Waters) with A-20 mM ammonium acetate containing 0.1% ace-tic acid in water, B-Acetonitrile as mobile phase with gradient mode at a flow rate of 0.3 mL/min. The developed method was validated for specificity, linearity, accuracy and precision in sausages samples. Linearity was over 0.998 with calibration curve of the mixed standards. The mean recoveries from sau-sages fortified at the level of 2.0∼10.0 mg/L were in range of 98.60∼109.16% with RSDs lower than 8.93%. The limits of detection (LOD) and the limits of quantification (LOQ) were in the range between 0.0003∼0.085 mg/L and 0.01∼0.257 mg/L, respectively. Intra-day precision and inter-day precision were 0.45∼6.16% and 2.81∼13.33%, respectively. Using presently developed determination method, 33 field sausage samples from Gwangju city in Korea were screened over nine preservatives. As a result, no preservatives were detected in all samples.
Abstract
A simultaneous determination method was developed for nine preservatives (benzoic acid, sorbic acid, dehydroacetic acid, methyl-, ethyl-, isopropyl-, propyl-, isobutyl- and butyl-parabens) in sausage by liq-uid chromatography with electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS). Each pa-rameter was established by multiple reaction monitoring in negative mode. Separation was achieved on a phenyl-hexyl (2.5 m, 2.1×150 mm, Waters) with A-20 mM ammonium acetate containing 0.1% ace-tic acid in water, B-Acetonitrile as mobile phase with gradient mode at a flow rate of 0.3 mL/min. The developed method was validated for specificity, linearity, accuracy and precision in sausages samples. Linearity was over 0.998 with calibration curve of the mixed standards. The mean recoveries from sau-sages fortified at the level of 2.0∼10.0 mg/L were in range of 98.60∼109.16% with RSDs lower than 8.93%. The limits of detection (LOD) and the limits of quantification (LOQ) were in the range between 0.0003∼0.085 mg/L and 0.01∼0.257 mg/L, respectively. Intra-day precision and inter-day precision were 0.45∼6.16% and 2.81∼13.33%, respectively. Using presently developed determination method, 33 field sausage samples from Gwangju city in Korea were screened over nine preservatives. As a result, no preservatives were detected in all samples.
참고문헌 (15)
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