食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
FOOD SAFETY AND QUALITY DETECTION TECHNOLOGY
2015年
8期
3262-3268
,共7页
吴振兴%静平%曹文卿%鲍蕾%梁成珠%宫小明
吳振興%靜平%曹文卿%鮑蕾%樑成珠%宮小明
오진흥%정평%조문경%포뢰%량성주%궁소명
海洋贝类%腹泻性贝毒毒素%高效液相色谱-电喷雾串联质谱法
海洋貝類%腹瀉性貝毒毒素%高效液相色譜-電噴霧串聯質譜法
해양패류%복사성패독독소%고효액상색보-전분무천련질보법
marine shellfish%diarrhetic shellfish poisoning toxins%high performance liquid chromatography-electrospray ionization mass spectrometry
目的:建立腹泻性贝毒毒素9种代表性化合物:大田软海绵酸、鳍藻毒素、蛤毒素2、扇贝毒素及其衍生物、环亚胺米氏裸甲藻毒素、螺环内酯毒素1和原多甲藻酸的高效液相色谱-电喷雾串联质谱(HPLC-ESI-MS/MS)检测方法。方法以80%甲醇水溶液对贝类组织中的毒素进行提取,再以亲水亲脂平衡柱(HLB)对提取液进行净化,最后以高效液相色谱-电喷雾串联质谱测定。结果 DSP毒素9种代表性化合物在各自浓度范围内线性良好,回收率为68.9%~94.2%,精密度为3.5%~9.5%。结论该方法具有灵敏度高、重现性好、操作简便、准确可靠等特点,适用于贝类中腹泻性贝毒毒素的测定。
目的:建立腹瀉性貝毒毒素9種代錶性化閤物:大田軟海綿痠、鰭藻毒素、蛤毒素2、扇貝毒素及其衍生物、環亞胺米氏裸甲藻毒素、螺環內酯毒素1和原多甲藻痠的高效液相色譜-電噴霧串聯質譜(HPLC-ESI-MS/MS)檢測方法。方法以80%甲醇水溶液對貝類組織中的毒素進行提取,再以親水親脂平衡柱(HLB)對提取液進行淨化,最後以高效液相色譜-電噴霧串聯質譜測定。結果 DSP毒素9種代錶性化閤物在各自濃度範圍內線性良好,迴收率為68.9%~94.2%,精密度為3.5%~9.5%。結論該方法具有靈敏度高、重現性好、操作簡便、準確可靠等特點,適用于貝類中腹瀉性貝毒毒素的測定。
목적:건립복사성패독독소9충대표성화합물:대전연해면산、기조독소、합독소2、선패독소급기연생물、배아알미씨라갑조독소、라배내지독소1화원다갑조산적고효액상색보-전분무천련질보(HPLC-ESI-MS/MS)검측방법。방법이80%갑순수용액대패류조직중적독소진행제취,재이친수친지평형주(HLB)대제취액진행정화,최후이고효액상색보-전분무천련질보측정。결과 DSP독소9충대표성화합물재각자농도범위내선성량호,회수솔위68.9%~94.2%,정밀도위3.5%~9.5%。결론해방법구유령민도고、중현성호、조작간편、준학가고등특점,괄용우패류중복사성패독독소적측정。
Objective To establish a high performance liquid chromatography (HPLC)-electrospray ionization mass spectrometry method for determination of 9 kinds of representative diarrhetic shellfish poisoning (DSP) toxins including okadaic acid(OA), dinophysistoxin1, 2(DTX1, DTX2), pectenotoxin2(PTX2), yessotoxin(YTX), homo-yessotoxin(hYTX), gymnodimine(GYM), spirolide1(SPX1) and azaspiracid1(AZA1) in shellfish. Methods The toxins were extracted with 80%methanol aqueous solution from the shellfish, then cleaned up by hydrophile-lipophile balance columns, at last, the extractive was determined by a reversed phase HPLC gradient program coupled with electrospray ionization mass spectrometry. Results Nine representative diarrhetic shellfish poisoning toxins had a good linear relationship in respective concentration range, the average recoveries were ranged from 68.9%~94.2%, and the precision was in ranged from 3.5%~9.5%. Conclusion The developed method is simple and accurate, which can be applied for determination of DSP toxins in shellfish.