宁波大学学报:理工版
寧波大學學報:理工版
저파대학학보:리공판
Journal of Ningbo University(Natural Science and Engineering Edition)
2011年
4期
25-28
,共4页
侯云丹%沈洁%徐继林%朱冬发%严小军
侯雲丹%瀋潔%徐繼林%硃鼕髮%嚴小軍
후운단%침길%서계림%주동발%엄소군
三疣梭子蟹%甲基法尼酯%气相色谱-盾谱联用
三疣梭子蟹%甲基法尼酯%氣相色譜-盾譜聯用
삼우사자해%갑기법니지%기상색보-순보련용
Portunus trituberculatus%methyl farnesoate%GC/MS
建立了人工养殖三疣梭子蟹(Portunus trituberculatus)淋巴和肌肉中甲基法尼酯的毛细管气相色谱.质谱联用检测法。向淋巴或冷冻干燥后的肌肉样品中加入十九烷酸甲酯作为定量内标物,淋巴中加入0.9%NaCl和乙腈后用正己烷提取;肌肉冷冻干燥后用正己烷提取,浓缩定容后用EI源在SIM检测模式下进行检测.结果表明:甲基法尼酯与内标物十九烷酸甲酯在SPB—1柱上得到良好的分离,方法在5.00~200.00ng·mL^-1。浓度范围内线性关系良好,相关系数为0.99995,方法的最低检测限3.27pg.淋巴和肌肉中甲基法尼酯平均回收率分别达到95.32%和88.37%,标准相对偏差分别为5.71%和7.94%.对采自浙江宁波象山港养殖三疣梭子蟹进行分析测定,甲基法尼酯在血清中含量在15.11~145.23ng·mL^-1。范围内,而肌肉中则在3.23~10.32ng·g^-1范围内.
建立瞭人工養殖三疣梭子蟹(Portunus trituberculatus)淋巴和肌肉中甲基法尼酯的毛細管氣相色譜.質譜聯用檢測法。嚮淋巴或冷凍榦燥後的肌肉樣品中加入十九烷痠甲酯作為定量內標物,淋巴中加入0.9%NaCl和乙腈後用正己烷提取;肌肉冷凍榦燥後用正己烷提取,濃縮定容後用EI源在SIM檢測模式下進行檢測.結果錶明:甲基法尼酯與內標物十九烷痠甲酯在SPB—1柱上得到良好的分離,方法在5.00~200.00ng·mL^-1。濃度範圍內線性關繫良好,相關繫數為0.99995,方法的最低檢測限3.27pg.淋巴和肌肉中甲基法尼酯平均迴收率分彆達到95.32%和88.37%,標準相對偏差分彆為5.71%和7.94%.對採自浙江寧波象山港養殖三疣梭子蟹進行分析測定,甲基法尼酯在血清中含量在15.11~145.23ng·mL^-1。範圍內,而肌肉中則在3.23~10.32ng·g^-1範圍內.
건립료인공양식삼우사자해(Portunus trituberculatus)림파화기육중갑기법니지적모세관기상색보.질보련용검측법。향림파혹냉동간조후적기육양품중가입십구완산갑지작위정량내표물,림파중가입0.9%NaCl화을정후용정기완제취;기육냉동간조후용정기완제취,농축정용후용EI원재SIM검측모식하진행검측.결과표명:갑기법니지여내표물십구완산갑지재SPB—1주상득도량호적분리,방법재5.00~200.00ng·mL^-1。농도범위내선성관계량호,상관계수위0.99995,방법적최저검측한3.27pg.림파화기육중갑기법니지평균회수솔분별체도95.32%화88.37%,표준상대편차분별위5.71%화7.94%.대채자절강저파상산항양식삼우사자해진행분석측정,갑기법니지재혈청중함량재15.11~145.23ng·mL^-1。범위내,이기육중칙재3.23~10.32ng·g^-1범위내.
An analytical method on sensitivity of methyl farnesoate in lymph and muscle of cultured Portunus trituberculatus is introduced using capillary gas chromatography-mass spectrometry. After nonadeeanoic acid methylester is added to lymph and frozen drying muscle as inner standard, and 0.9% NaCl and acetonitrile are added to lymph, methyl farnesoate can be extracted with n-hexane effectively, and determined using EI-SIM-MS after concentration. The results indicate that methyl farnesoate and the inner standard can be separated from each other on SBP-1 column with sharp peak. The linearity is agreeable from 5.00 to 200.00ng.mL^-1 and relative coefficient is found to be 0.999 95, with low detection limit of 3.27 pg. The average recovery rate in lymph and muscle is 95.32% and 88.37%, respectively, and the standard deviation reads 5.71% and 7.94%, respectively. This method is applied to determine the methyl farnesoate at different stages of P trituberculatus, coming up with the results of 15.11-145.23 ng.mL^-1 in lymph and 3.23-10.32 ng.g^-1 in muscle.