LC-MS/MS를 이용한 패류 및 피낭류 중 마비성 패류독소 분석법의 유효성 검증
Validation of LC-MS/MS Method for Analysis of Paralytic Shellfish Toxins in Shellfish and Tunicates
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초록
The mouse bioassay has been used widely for the monitoring of paralytic shellfish toxins (PSTs) in many countries. However, this method shows low sensitivity and high limit of detection (LOD), as well as it cannot confirm toxic profiles. Recently, LC-MS/MS method was studied for the quantitative of PSTs, however, the method has any problemswith unstable retention times by ionization suppression caused by high salt concentration in shellfish extracts. Toestablish an alternative method for PSTs analysis, we tried to original LC-MS/MS methods adding desalting operationusing amorphous graphitized polymer carbon solid-phase extraction cartridges. The method validation was conductedto determine linearity, limit of detection, limit of quantification (LOQ), accuracy, and precision in quantifyingPSTs. The correlation coefficients for all tested PSTs maintained over 0.999. The LODs and LOQs for all PSTs wereabout 0.19-1.05 μg/kg and 0.58-3.18 μg/kg, respectively. The accuracies for PSTs were 95.4-107.7% for saxitoxingroup, 97.1-100.9% for gonyautoxin group, 99.0-100.8% for N-sulfocarbamoyl toxin group, and 96.8-104.6% fordecarbamoyl toxin group. These results indicate that the modified LC-MS/MS method was appropriate for analyzingthe PSTs in shellfish and tunicates.
Abstract
The mouse bioassay has been used widely for the monitoring of paralytic shellfish toxins (PSTs) in many countries. However, this method shows low sensitivity and high limit of detection (LOD), as well as it cannot confirm toxic profiles. Recently, LC-MS/MS method was studied for the quantitative of PSTs, however, the method has any problemswith unstable retention times by ionization suppression caused by high salt concentration in shellfish extracts. Toestablish an alternative method for PSTs analysis, we tried to original LC-MS/MS methods adding desalting operationusing amorphous graphitized polymer carbon solid-phase extraction cartridges. The method validation was conductedto determine linearity, limit of detection, limit of quantification (LOQ), accuracy, and precision in quantifyingPSTs. The correlation coefficients for all tested PSTs maintained over 0.999. The LODs and LOQs for all PSTs wereabout 0.19-1.05 μg/kg and 0.58-3.18 μg/kg, respectively. The accuracies for PSTs were 95.4-107.7% for saxitoxingroup, 97.1-100.9% for gonyautoxin group, 99.0-100.8% for N-sulfocarbamoyl toxin group, and 96.8-104.6% fordecarbamoyl toxin group. These results indicate that the modified LC-MS/MS method was appropriate for analyzingthe PSTs in shellfish and tunicates.
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