采用改良的方法从贻贝肝胰腺中提取与净化麻痹性贝毒

Improved Methods for Extraction and Cleanup of Paralytic Shellfish Toxins From Mussel Hepatopancreas

建立简单有效的方法从贝类肝胰腺中提取和净化麻痹性贝类毒素。采用体积分数为1％醋酸在超声、加热及不同的加热时间条件下提取PSP毒素，提取效果与0．1mol／LHCl的提取效果进行比较。为避免毒素纯化过程中粗提液中杂质对分离纯化柱的污染和堵塞，研究中分别利用二氯甲烷、正丁醇和活性炭，对在最适提取条件下获得的PSP粗提液进行净化处理。实验结果表明，采用体积分数为1％醋酸溶液在76℃水浴中浸提30rain既能保证绝大部分毒素组分被提取出来又能保证各毒素组分的含量；二氯甲烷净化效果较正丁醇好，它能有效去除粗提液中部分脂类物质，净化后各毒素组分回收率为104％～151％；采用活性炭吸附脱附的方式能进一步去除经二氯甲烷净化后的粗提液中的杂质，尽管有些毒素的回收率有所降低，但大多数毒素的回收率在80％以上。

The ultimate goal of this study is to develop simple and effective methods for extraction and cleanup of PSP toxins from the hepatopancreas of mussels. Different extraction procedures using 1 ; acetic acid were tested, including 3 time periods vs sonication at 13 ;C; results were compared to extraction in 0.1 mmol/L HC1 at 76 ;C for 10 min. Cleanup is required to remove impurities that contaminate separation columns in the process of purification. Cleanup procedures were tested on the extracts obtained using the best extraction procedure. Recovery percentage is reported relative to this treatment. The results showed that dichloromethane （CH2 C12） exhibited better clean-up effect than n-butanol, increasing recovery rates to 104 %-151%. Impurities in the CH2 Cl2-cleaned-up extract could be removed further by activated car- bon adsorption-desorption method. After this step, some toxins reduced somewhat, but the recovery rates of most of PSP toxins were from 80% to 112%.