多壁碳纳米管固相萃取-超高效液相色谱串联质谱法测定织纹螺中河豚毒素

Determination of tetrodotoxin in Nassarius by ultra high performance liquid chromatography-tandem mass spectrometry with multi-walled carbon nanotubes purification

建立了多壁碳纳米管(MWCNTs)固相萃取-超高效液相色谱串联质谱法(UPLC-MS/MS)测定织纹螺中河豚毒素(TTX)的方法,样品用1%乙酸甲醇溶液提取,调节pH至8.5~9.0后,采用碳纳米管净化处理后上机测定。以乙腈和0.1%甲酸水溶液为流动相,经Amide柱梯度洗脱,以电喷雾离子源正离子模式,多反应监测(MRM)测定,外标法定量。在0.3~50 ng·mL^(–1)质量浓度范围内,相关系数(R)大于0.999,加标回收率为83.7%~91.4%,相对标准偏差为2.3%~8.6%,检测限和定量限分别为0.3μg·kg^(–1)和1μg·kg^(–1)。该方法适用于织纹螺中TTX的检测。

A sensitive and reliable method for determination of tetrodotoxin(TTX)in Nassarius was established using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The sample was extracted by 1%acetic acid-methanol solution,then the pH value was adjusted to 8.5?9.0.After purification with multi-walled carbon nanotubes(MWCNTs),the sample was subjected to an analytical procedure.The mobile phase containing acetonitrile and 0.1%formic acid solution with a linear gradient elution was utilized to separate TTX on an Amide column.The quantitative analysis was carried out with an external standard method in the multiple reaction monitoring mode using positive electrospray ionization.The calibration curve for TTX was linear(R>0.999)from 0.3 ng·mL^–1 to 50 ng·mL^–1.The recoveries were 83.7%?91.4%with the RSDs of 2.3%?8.6%.The limits of detection and quantification were 0.3μg·kg^–1 and 1μg·kg^–1,respectively.This method is suitable for determination of TTX in Nassarius.