论文部分内容阅读
目的建立了测定贝类中大田软海绵酸(OA)、鳍藻毒素(DTX1、DTX2)、紫贻贝毒素(YTX)、原多甲藻酸贝毒素(AZA1)、螺环内酯毒素(SPX1)6种脂溶性贝类毒素的固相萃取-高效液相色谱-串联质谱方法。方法匀浆贝类组织,用80%甲醇提取,Strata~(TM)-X固相萃取小柱净化,0.3%氨水甲醇溶液洗脱,离心超滤管离心纯化。采用XTerra MS C_(18)柱(150 mm×2.1 mm,35μm)分离,以含6.7 mmol/L氨水的90%乙腈-水溶液为流动相进行梯度洗脱,选择多反应监测模式检测,正、负离子切换扫描,基质标准校正外标法定量。结果 6种脂溶性贝类毒素的定量限为0.2~1.0μg/kg,在相应浓度范围内线性良好,相关系数均>0.995;低、中、高3个添加水平的平均加标回收率在78.8%~116%之间;相对标准偏差(RSD)为3.8%~14.5%。应用建立的方法对多份贝类样品进行分析,均未检出目标组分。结论方法选择性、灵敏性和准确度高,适用于贝类产品中脂溶性贝类毒素的确证及定量分析。
OBJECTIVE To establish a method for the determination of salicylic acid (OA), tryptoxin (DTX1, DTX2), mussel toxin (YTX), azadirachtin (AZA1), spironolactone toxin ) Six kinds of fat - soluble shellfish toxins by solid phase extraction - high performance liquid chromatography - tandem mass spectrometry method. Methods The shellfish tissues were homogenized, extracted with 80% methanol, cleaned up with Strata ™ -X solid phase extraction cartridges, eluted with 0.3% ammonia solution and centrifuged. Separation was performed on a XTerra MS C 18 column (150 mm × 2.1 mm, 35 μm) using a gradient elution of 90% acetonitrile-water containing 6.7 mmol / L aqueous ammonia as the mobile phase. The multi-reaction monitoring mode was used to detect the positive and negative ions Switch scan, matrix standard calibration external standard method. Results The limit of quantitation of six kinds of liposoluble molluscan shellfish toxins was 0.2-1.0 μg / kg, with good linearity in the corresponding range of concentration, the correlation coefficients were both> 0.995. The average recoveries of the three kinds of liposoluble molluscan shellfish toxins at 78.8 % ~ 116%; The relative standard deviation (RSD) was 3.8% ~ 14.5%. Multiple shellfish samples were analyzed using the established method. None of the target components were detected. Conclusion The method is selective, sensitive and accurate. It is suitable for the confirmation and quantitative analysis of liposoluble shellfish toxins in shellfish products.