超高效液相色谱-四极杆串联线性离子阱质谱法测定贝类中的脂溶性贝类毒素  

Determination of lipophilic marine biotoxins in shellfish foods by ultra performance liquid chromatography-hybrid triple quadrupole linear ion trap-mass spectrometry

作　　者：刘红河[1] 秦逍云[1] 廖仕成[1] 康莉[1] 毛丽莎[1] 肖惠贞[2] 尹江伟[2] Liu Honghe;Qin Xiaoyun;Liao Shicheng;Kang Li;Mao Lisha;Xiao Huizhen;Yin Jiangwei(Shenzhen Center for Disease Control and Prevention,Shenzhen 518055,China;Baoan District Center for Disease Control and Prevention,Shenzhen 518101,China)

机构地区：[1]深圳市疾病预防控制中心,深圳518055 [2]深圳市宝安区疾病预防控制中心,深圳518101

出　　处：《卫生研究》2021年第6期967-974,共8页Journal of Hygiene Research

基　　金：科技部国家重点研发计划(No.2019YFC1605103,2019YFC1605104);深圳市医学重点学科建设经费资助(No.SZXK066)。

摘　　要：目的建立一种超高效液相色谱-四极杆串联线性离子阱质谱技术测定贝类食品中12种脂溶性贝类毒素的方法。方法贝类中12种脂溶性贝类毒素采用甲醇超声提取,经Strata-X固相萃取小柱净化,用含0.3%(V/V)氨水的甲醇洗脱后,0.22μm微孔滤膜过滤,经Waters ACQUITY UPLC BEH C_(18)(150 mm×2.1 mm,1.7μm)超高效液相色谱柱分离,选用乙腈-水(含0.01%氨水和2 mmol/L甲酸铵)为流动相,梯度洗脱分离12种脂溶性贝类毒素;在优化的串联四极杆质谱条件下,采用电喷雾电离源、正负离子同时扫描模式、多反应监测方式,外标法定量,采用信息依赖采集扫描功能结合增强子离子扫描模式对检出阳性结果进行定性分析。结果方法的线性范围为0.5~50μg/L,12种脂溶性贝类毒素在各种样品基质中均有良好的线性关系,相关系数(r)在0.9984~0.9999,方法检出限为0.15~0.29μg/kg;方法回收率为80.0%~116.0%,相对标准偏差为0.6%~6.4%(n=7)。结论该方法测定12种脂溶性贝类毒素的残留量简便、快速、定性准确,可以满足对贝类食品中脂溶性贝类毒素的监测要求。OBJECTIVE An ultra performance liquid chromatography-hybrid triple quadrupole linear ion trap-mass spectrometry(UPLC-QqLIT-MS)was established for determination of lipophilic marine biotoxins in shellfish.And the 12 lipophilic marine biotoxins in shellfish were surveyed.METHODS The lipophilic marine biotoxins in homogenized shellfish were ultrasonically extracted by methanol in super-sonic instrument,and cleaned up by solid phase extraction of Strata-X column,and eluted with methanol(containing 0.3%ammonia water).The elution was diluted with water,and cleaned by 0.22μm millipore filter.The filtrate was separated on a Waters ACQUITY UPLC BEH C_(18) column(150 mm×2.1 mm,1.7μm)by gradient elution in 12 minutes with acetronitrilewater(containing 0.01%(V/V)ammonia and 2 mmol/L ammonium formate)as mobile phase,and detected by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),identified by electrospray ionization(ESI)in simultaneous scanning mode of positive and negative ions using multiple reaction monitoring,and quantified with external standards.Information dependent acquisition scan function(IDA)combined with enhanced production scan(EPI)was used to confirm the 12 lipophilic marine biotoxins.RESULTS The calibration curves of 12 lipophilic marine biotoxins showed good linearity in the range of 0.5-50μg/L with correlation coefficients were 0.9984-0.9999.The detection limits of the method were 0.15-0.29μg/kg.The recoveries of three spiking levels ranged from 80.0%to 116.0%,and the relative standard deviation(RSD)were 0.6%-6.4%(n=7).CONCLUSION The method for determination of 12 lipophilic marine biotoxins in shellfish by UPLC-QqLIT-MS was of operation convenience,less interference from impurities and good accuracy,which could meet the requirements for the determination of 12 lipophilic marine biotoxins residues in sea foods.

关 键 词：脂溶性贝类毒素 四极杆串联线性离子阱质谱 贝类 

分 类 号：R155.51[医药卫生—营养与食品卫生学]