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液相色谱-串联质谱检测贝类组织中5种脂溶性贝毒素 被引量:17
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作者 姚建华 谭志军 周德庆 《分析化学》 SCIE EI CAS CSCD 北大核心 2010年第12期1714-1720,共7页
建立了液相色谱-串联质谱分析贝类组织中米氏裸甲藻(GYM)贝毒素、螺环内酯毒素(SPX1)、大田软骨酸(OA)贝毒素、蛤毒素(PTX2)、原多甲藻酸(AZA1)贝毒素的方法。用甲醇-水(4:1,V/V)溶液对贝类组织中GYM,SPX1,OA,PTX2和AZA1进行提取,MAX阴... 建立了液相色谱-串联质谱分析贝类组织中米氏裸甲藻(GYM)贝毒素、螺环内酯毒素(SPX1)、大田软骨酸(OA)贝毒素、蛤毒素(PTX2)、原多甲藻酸(AZA1)贝毒素的方法。用甲醇-水(4:1,V/V)溶液对贝类组织中GYM,SPX1,OA,PTX2和AZA1进行提取,MAX阴离子交换柱净化后,采用液相色谱分离,除OA以负离子选择反应监测外,GYM,SPX1,PTX2和AZA1以电喷雾离子源正离子选择反应监测模式进行质谱分析。5种脂溶性贝毒素GYM,SPX1,OA,PTX2和AZA1在各自相应浓度范围内线性良好,相关系数>0.99。扇贝闭壳肌空白样品添加5种贝毒素的提取率均为78.6%~94.4%(n=6);精密度(RSD)为6.8%~14.9%。贝类组织中5种贝毒素GYM,SPX1,OA,PTX2和AZA1的检出限分别为0.10,0.21,2.00,0.32和0.04μg/kg。 展开更多
关键词 脂溶性贝毒素 贝类组织 液相色谱-串联质谱
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同位素内标稀释液相色谱-串联质谱法测定鱼贝类组织中残留的环丙氟哌酸 被引量:7
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作者 陈晓红 王玉飞 +1 位作者 姚浔平 金米聪 《色谱》 CAS CSCD 北大核心 2009年第1期39-43,共5页
建立了不同鱼贝类肌肉组织中以氘代同位素为内标测定环丙氟哌酸残留量的液相色谱-串联质谱(LC—MS/MS)方法。样品加入内标环丙氟哌酸-D8和磷酸盐缓冲溶液(pH7.0)后进行匀质并用乙腈超声提取,经正己烷脱脂后采用Waters Oasis'MA... 建立了不同鱼贝类肌肉组织中以氘代同位素为内标测定环丙氟哌酸残留量的液相色谱-串联质谱(LC—MS/MS)方法。样品加入内标环丙氟哌酸-D8和磷酸盐缓冲溶液(pH7.0)后进行匀质并用乙腈超声提取,经正己烷脱脂后采用Waters Oasis'MAX小柱净化,在Cloversil—C18柱上,以乙腈-0.05%三氟醋酸(体积比为25:75)为流动相,采用多反应监测(MRM)模式,液相色谱-电喷雾质谱法测定。根据环丙氟哌酸和氘代内标物的定量离子质量色谱图的峰面积比值,采用内标法定量。结果表明,环丙氟哌酸和内标的定量离子峰面积比值与环丙氟哌酸浓度在0.1~50.0μg/kg范围内呈现良好的线性关系,相关系数为0.9991,方法的定量检测限为0.1μg/kg,回收率为92.5%~98.1%,相对标准偏差(RSD)小于4.3%。将该方法用于市场上10种鱼和贝类样品的检测,结果表明该法具有灵敏、准确的优点,完全满足残留分析的确证检测要求。 展开更多
关键词 固相萃取 液相色谱-串联质谱法 同位素内标 环丙氟哌酸 贝类组织
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Studies on the Time of Accumulation and Elimination of Alexandrium tamarense Toxins in Argopectens irradias
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作者 Chunjiang Guan Hao Guo +2 位作者 Xiaoyang Jiao Wen Zhao Hongbo Li 《Journal of Earth Science and Engineering》 2012年第2期112-117,共6页
Using a PSP (paralytic shellfish poisoning) toxin-producing strain of4lexandrium tamarense, it studied the timing of toxin accumulation and elimination of PSP toxins in Argopectens irradias. The PSP toxicity was stu... Using a PSP (paralytic shellfish poisoning) toxin-producing strain of4lexandrium tamarense, it studied the timing of toxin accumulation and elimination of PSP toxins in Argopectens irradias. The PSP toxicity was studied by following the standard PSP mouse bioassay developed by the Association of Official Analytical Chemists (AOAC). Alexandrium tamarense was cultured to an average density of 1.26 × 10^4/mL for a total of about 50 L culture. The toxicity of the alga was 2.18 ×10^-6 MU/cell. The results show that PSP content increased with time in both visceral and muscle tissue during a two-week accumulation period during which scallops were fed with ,4. tamarense. The average toxin level in scallop's viscera was 49.4 MU/g, with an average of 10.0 MU/g in muscle tissue. This level is 2.5 times higher than the sanitation standard (4.0 MU/g of muscles). The highest value was 61.0 MU/g in the viscera. In summary, the viscera accumulated greater concentrations of toxin than muscle tissue. Scallops that had accumulated toxins were transplanted for two weeks into a field environment containing no toxic algae. The PSP content of the scallops decreased to 7.9 MU/g viscera and 1.6 MU/g muscles two weeks after being transplanted, but did not reach the sanitation standard. Under the experimental conditions, the toxin depuration rate of shellfish toxin was 12% daily. This study worked toward the development of a sanitary shellfish industry and better management of PSP toxin-impacted shellfish in China. 展开更多
关键词 PSP argopectens irradias accumulation and elimination time.
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