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《化学分析计量》 2019年增刊
DOI:10.3969/j.issn.1008-6145.2019.z1.005
超高效液相色谱-串联质谱法测定贝类中8 种脂溶性贝类毒素
冯静1,王超2,华正罡1
1. 辽宁省疾病预防控制中心,沈阳 110005; 2. 辽宁省检验检测认证中心,沈阳 110036 
Determination of 8 fat soluble shellfish toxins by UPLC-MS/MS
FENG Jing1, WANG Chao2, HUA Zhenggang1
1. Liaoning Center for Disease Control and Prevention, Shenyang 110005, China;
2. Liaoning Inspection Examination and Certification Centre, Shenyang 110036, China 
摘要:建立超高效液相色谱-串联质谱法测定贝类中脂溶性贝类毒素。样品组织经100% 甲醇提取过滤后直接进样用于测定游离态的原多甲藻酸毒素(AZA1,AZA2 和AZA3)、大田软海绵酸(OA)、鳍藻毒素(DTX2,DTX1和PTX2)、虾夷扇贝类毒素(YTX)。采用碱水解乙酰化OA 和DTXs 转化成游离的OA,DTX1 及DTX2,测定OA类毒素总含量。色谱柱为Waters UPLC BEH C18 柱(50 mm×2.1 mm,1.7 μm),流动相A 相为甲酸-甲酸铵缓冲液(50 mmol/L 甲酸溶液-2 mmol/L 甲酸铵溶液),B 相为酸化乙腈(95% 乙腈水溶液,含50 mmol/L 甲酸溶液和2 mmol/L 甲酸铵溶液),梯度洗脱,流量为0.3 mL/min,进样体积为10 μL,多反应监测(MRM)模式检测。最低检出限AZA1,AZA2,AZA3 为5μg /kg ;OA,DTX2,DTX1,PTX2,YTX 为10 μg /kg。线性范围为2.5~100 μg/L,线性相关系数均大于0.995。平均回收率为91.3%,测定结果的相对标准偏差为1.7%(n=6)。该方法检出限低,精密度高,适用于贝类中脂溶性贝类毒素的检测。 
Abstract:An ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was established for the determination of 8 fat soluble shellfish toxins. The samples after 100% methanol extraction was direct determination of the original fat soluble shellfish toxins as proto-polyalginate toxin AZA1, AZA2, AZA3; okadaic acid(OA), fin algae toxin DTX2, DTX1, PTX2; and yessotoxins(YTX). The total OA was determined by conversion of OA and DTXs to absolute OA, DTX1 and DTX2 with alkali hydrolysis and acetylation. The chromatographic column was Waters UPLC BEH C18(50 mm×2.1 mm, 1.7 μm), gradient elution method was selected, A phase of mobile phase was 50 mmol/L formic acid-2 mmol/L ammonium formate solution, B phase was 95% acetonitrile aqueous solution (containing 50 mmol/L formic acid and 2 mmol/L ammonium formate), the flow rate was 0.3 mL/min, the injection volume was 10 μL, and determination was performed under multiple reaction monitoring mode. The LODs of AZA1, AZA2, AZA3 were 5 μg/kg; the LODs of OA, DTX2, DTX1, PTX2 and YTX were 10 μg/kg. The linear range was 2.5-100 μg/L, and the linear correlation coefficient was more than 0.995. The average recoveries was 91.3% with the relative deviation of 1.7% (n=6). The method has low detection limit, high precision. and it is suitable for determination of 8 fat soluble shellfish toxins. 
关键词:超高效液相色谱-串联质谱法;贝类;脂溶性贝类毒素 
Keywords:UPLC-MS/MS; shellfish; fat soluble shellfish toxins 
本文引用格式:
冯静,王超,华正罡. 超高效液相色谱- 串联质谱法测定贝类中8 种脂溶性贝类毒素[J]. 化学分析计量,2019,28(Z1):23-27.
FENG J,WANG C,HUA Z G. Determination of 8 fat soluble shellfish toxins by UPLC-MS/MS[J]. Chemical analysis and meterage,2019,28(Z1)23-27. 

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