LC-MS/MS (Liquid Chromatography-Tandem Mass Spectrometry)를 이용한 패류 및 피낭류 중 아자스필산 분석법의 유효성 검증
Verification of Analytical Method of Azaspiracid Toxins in Shellfish and Tunicates by Liquid Chromatography-Tandem Mass Spectrometry
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초록
Although, mouse bioassay for the monitoring of azaspiracids (AZAs) toxins in shellfish has been used previously, the reported method has low sensitivity and it is time-consuming. Recently, there is an interest in the quantitative analysis of AZAs using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The purpose of this study is to verify the simultaneous analysis of AZAs in shellfish and tunicate in Korea using LC-MS/MS. To validate the method, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, and repeatability were determined. All standard compounds were analyzed within 7 min. The correlation coefficients (R2) of the standard solution was higher than 0.9995 (within the range of 0.8-10.0 μg/L). The LODs and LOQs of AZAs in shellfish were 0.08-0.16 μg/kg and 0.23-0.50 μg/kg, respectively. The accuracy and precision of the method for determining AZAs in shellfish were 87.1-93.0% and 1.23-4.91%, respectively. Consequently, the verified LC-MS/MS method is suitable to analyze AZAs in shellfish and tunicates in Korea.
Abstract
Although, mouse bioassay for the monitoring of azaspiracids (AZAs) toxins in shellfish has been used previously, the reported method has low sensitivity and it is time-consuming. Recently, there is an interest in the quantitative analysis of AZAs using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The purpose of this study is to verify the simultaneous analysis of AZAs in shellfish and tunicate in Korea using LC-MS/MS. To validate the method, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, and repeatability were determined. All standard compounds were analyzed within 7 min. The correlation coefficients (R2) of the standard solution was higher than 0.9995 (within the range of 0.8-10.0 μg/L). The LODs and LOQs of AZAs in shellfish were 0.08-0.16 μg/kg and 0.23-0.50 μg/kg, respectively. The accuracy and precision of the method for determining AZAs in shellfish were 87.1-93.0% and 1.23-4.91%, respectively. Consequently, the verified LC-MS/MS method is suitable to analyze AZAs in shellfish and tunicates in Korea.
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