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目的神经性贝类毒素(NSP)目前的检测方法主要为小鼠生物分析法[1]。建议对该方法做适当地修订,明确旋转蒸馏的真空度压强在200 KPa及其以下,或以新建立的气相色谱法测定方法作为评估二氯甲烷溶剂残留对最终结果影响的附属方法,以避免二氯甲烷溶剂对最终结果的影响,保证最终结果的准确性。方法用乙酸乙酯作为样品提取液中二氯甲烷的萃取溶剂,并建立相应的气相色谱方法测定样品中残留的二氯甲烷。结果试验表明采用不同真空度旋转蒸馏提取液时,其二氯甲烷溶剂残留量是明显不同的。当旋转蒸馏的真空度压强在200 KPa及其以下时,提取液中残留的二氯甲烷量才对最终结果影响极小,可以忽略。结论样品中的二氯甲烷残存量与旋转蒸发仪的旋转真空压强有直接关系。这是由于样品对二氯甲烷溶剂存在一定的吸附作用力。当旋转蒸馏真空度没有达到一定要求,仍然会在样品中吸附一定量的二氯甲烷残留,并对结果造成较大影响,直接影响结果的准确性。
The current detection method of neuropathic shellfish toxin (NSP) is mainly mouse bioanalysis [1]. It is recommended that this method be properly revised to clarify that the vacuum pressure of rotary distillation is at or below 200 KPa or that a newly established gas chromatographic method be used as an adjunct method to assess the effect of residual solvent on methylene chloride on the end result to avoid Methylene chloride solvent on the final result, to ensure the accuracy of the final result. Methods Ethyl acetate was used as the extraction solvent of methylene chloride in the sample extract, and the corresponding gas chromatographic method was established to determine the residual dichloromethane in the sample. The results show that using different degrees of vacuum rotary distillation extract, the solvent residue of methylene chloride is significantly different. When the pressure of vacuum distillation in rotary distillation is below 200 KPa, the amount of methylene chloride remaining in the extract has little effect on the final result and can be neglected. Conclusion The residual amount of methylene chloride in the sample is directly related to the rotary vacuum pressure of the rotary evaporator. This is because the sample has a certain adsorption force on the methylene chloride solvent. When the degree of vacuum in rotary distillation does not meet the requirements, a certain amount of dichloromethane residue will still be adsorbed in the sample and the result will be greatly affected, which will directly affect the accuracy of the result.