|
|
|
| Determination of tetrodotoxin in salted pufferfish by liquid chromatography-tandem mass spectrometry |
| YU Sha, XU Meijia, XU Xiaomin
|
| Department of Physicochemical and Toxicology, Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, Zhejiang 310051, China |
|
|
|
|
Abstract Objective To develop a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method with cation exchange-based solid phase extraction (SPE) for determination of tetrodotoxin (TTX) in salted pufferfish. Methods Evenly crushed salted pufferfish samples were subjected to ultrasound-assisted extraction with 0.5% acetic acid/50% methanol/water. The extract was cleaned with cation exchange-based SPE cartridge and eluted with 0.3% hydrochloric acid and 50% acetonitrile/water. The eluent was neutralized with ammonia and separated with a Waters XBridgeTM BEH Amide column (150 mm×3.0 mm, 1.7 μm), and determined using LC-MS/MS in a multiple reaction monitoring mode. Results The matrix effects of TTX were 85.7%-92.4%, and the matrix suppression effect was under effective control following clean-up procedures using the optimized SPE method. The TTX showed a good linear relationship at the range of 2.0 to 4 000 μg/kg, with a correlation coefficient (r2) of 0.999 2. The limits of detection and quantitation for TTX in sample matrix were 1.0 μg/kg and 2.0 μg/kg, respectively. The mean spiked-recovery rates were 81.2% to 96.5% at spiked amounts of 2.0, 200 μg/kg and 2 200 μg/kg, with relative standard deviations (RSDs) of 4.3% to 7.5%. The intraday accuracy and precision of TTX were 84.4% to 95.6% and 4.9% to 5.8% in quality control samples, and the interday accuracy and precision of TTX were 86.1% to 94.9% and 5.5% to 8.5% in quality control samples. The detection of TTX was 60.5% in 38 market-sold salted pufferfish products using the established LC-MS/MS method. Conclusion The established LC-MS/MS method is effective for accurate quantitative determination of TTX in salted pufferfish.
|
|
Received: 17 April 2023
Revised: 31 May 2023
Published: 17 July 2023
|
|
|
|
|
|
[1] GUARDONE L,MANESCHI A,MEUCCI V,et al.A global retrospective study on human cases of tetrodotoxin(TTX)poisoning after seafood consumption[J].Food Rev Int,2020,36(7):645-667.
[2] 杨双喜,张立军,朱永平,等.宁波市售鲜活海产品河豚毒素污染现状及评价[J].浙江预防医学,2014,26(10):1007-1009.
[3] KATIKOU P,GOKBULUT C,KOSKER A R,et al.An updated review of tetrodotoxin and its peculiarities[J/OL].Mar Drugs,2022,20[2023-05-31].https://doi.org/10.3390/md20010047.
[4] LI Y,XU X,LIU L,et al.A gold nanoparticle-based lateral flow immunosensor for ultrasensitive detection of tetrodotoxin[J].Analyst,2020,145(6):2143-2151.
[5] MAN C N,NOOR N M,HARN G L,et al.Screening of tetrodotoxin in puffers using gas chromatography-mass spectrometry[J].J Chromatogr A,2010,1217(47):7455-7459.
[6] YASUMOTO T,TOORU M.Fluorometric determination of tetrodotoxin by high performance liquid chromatography[J].Agric Biol Chem,1985,49(10):3077-3080.
[7] HU C,ZHANG Y,ZHOU Y,et al.Tetrodotoxin and its analogues in food:recent updates on sample preparation and analytical methods since 2012[J].J Agric Food Chem,2022,70(39):12249-12269.
[8] HORT V,ARNICH N,GUERIN T,et al.First detection of tetrodotoxin in bivalves and gastropods from the french mainland coasts[J/OL].Toxins(Basel),2020,12(9)[2023-05-31].https://doi.org/10.3390/toxins12900599.
[9] 张晓艺,张秀尧,蔡欣欣,等.温州市织纹螺麻痹性贝类毒素和河豚毒素检测结果分析[J].预防医学,2019,31(9):936-939.
[10] TURNER A D,DHANJI-RAPKOVA M,FONG S Y T,et al.Ultrahigh-performance hydrophilic interaction liquid chromatography with tandem mass spectrometry method for the determination of paralytic shellfish toxins and tetrodotoxin in mussels,oysters,clams,cockles,and scallops:collaborative study[J].J AOAC Int,2020,103(2):533-562.
[11] 中华人民共和国农业农村部.鲜、冻养殖河豚鱼:SC/T 3124—2019[S].2019.
[12] 张秀尧,蔡欣欣,张晓艺,等.二维超高效液相色谱-三重四极杆/复合线性离子阱质谱联用法快速测定水产品及其制品中河豚毒素[J].食品科学,2020,41(18):311-316.
[13] XU X M,YU X W,LU M,et al.Study of the matrix effects of tetrodotoxin and its content in cooked seafood by liquid chromatography with triple quadrupole mass spectrometry[J].J Sep Sci,2015,38(19):3374-3382.
[14] REVERTE L,RAMBLA-ALEGRE M,LEONARDO S,et al.Development and validation of a maleimide-based enzyme-linked immunosorbent assay for the detection of tetrodotoxin in oysters and mussels[J].Talanta,2018,176:659-666.
[15] JEN H C,LIN S J,TSAI Y H,et al.Tetrodotoxin poisoning evidenced by solid-phase extraction combining with liquid chromatography-tandem mass spectrometry[J].J Chromatogr B,2008,871(1):95-100.
[16] 达情,刘伟,沈保华,等.液相色谱-串联质谱法分析生物检材中的河豚毒素[J].法医学杂志,2010,26(6):432-435.
[17] 严忠雍,张小军,李奇富,等.免疫亲和柱净化-液相色谱-串联质谱法测定海洋生物中河豚毒素[J].分析化学,2015,43(2):277-281. |
|
|
|
