超高效液相-飞行时间质谱法测定郫县豆瓣中的亚精胺
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摘要
该研究建立了一种超高效液相-飞行时间质谱仪串联技术测定亚精胺的方法。结果表明:在正离子采集模式下,去簇电压为60 V,碰撞电压为20 V的条件下,测定方法有较好的准确度和灵敏度。亚精胺在0.5～10.0 mg/L浓度范围内线性良好(相关系数R~2=0.9989),方法检测限为0.031 mg/kg,加标回收率范围为92.65%～100.58%,精密度范围为1.01%～2.98%,|基质效应|<20%。利用此方法分别对10种商业郫县豆瓣酱的亚精胺含量进行测定,发现10种豆瓣酱中均有亚精胺检出。该方法准确性好、灵敏度高且重现性好,为郫县豆瓣酱中亚精胺含量的研究提供了一种检测手段。
A method of ultra-high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UHPLC-Q-TOF) for detecting spermidine levels is established. The results show that the method has better accuracy and sensitivity under the conditions of 60 V declustering potential and 20 V collision energy in the positive ion collection mode. The linearity of spermidine is good in the concentration range of 0.5～10.0 mg/L with the correlation coefficient R~2=0.9989. The detection limit is 0.031 mg/kg, the recovery rate is 92.65%～100.58% with the relative standard deviation of 1.01%～2.98%, and the |matrix effect| is less than 20%. Based on this method, the spermidine content of 10 kinds of commercial Pixian bean paste is detected. The results indicate that this method is sensitive, efficient and accurate, it is suitable for the simultaneous determination of spermidine content in Pixian bean paste.
A method of ultra-high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UHPLC-Q-TOF) for detecting spermidine levels is established. The results show that the method has better accuracy and sensitivity under the conditions of 60 V declustering potential and 20 V collision energy in the positive ion collection mode. The linearity of spermidine is good in the concentration range of 0.5～10.0 mg/L with the correlation coefficient R~2=0.9989. The detection limit is 0.031 mg/kg, the recovery rate is 92.65%～100.58% with the relative standard deviation of 1.01%～2.98%, and the |matrix effect| is less than 20%. Based on this method, the spermidine content of 10 kinds of commercial Pixian bean paste is detected. The results indicate that this method is sensitive, efficient and accurate, it is suitable for the simultaneous determination of spermidine content in Pixian bean paste.
引文
[1]李幼筠.“郫县豆瓣”剖析[J].中国酿造,2008,27(11):19-23.
[2]Jose Maria Landete,Rosario Munoz.Characterization of a second ornithine decarboxylase isolated from Morganella morganii[J].Journal of Food Protection,2008,71(3):657.
[3]Kalac P.Health effects and occurrence of dietary polyamines:a review for the period 2005-mid 2013[J].Food Chemistry,2014,161(11):27-39.
[4]Madeo F,Eisenberg T,Pietrocola F,et al.Spermidine in health and disease[J].Science,2018,359(6374):2788.
[5]Morselli E,Mariňo G,Bennetzen M V,et al.Spermidine and resveratrol induce autophagy by distinct pathways converging on the acetylproteome[J].Journal of Cell Biology,2011,192(6):615-629.
[6]Eisenberg T,Knauer H,Schauer A,et al.Induction of autophagy by spermidine promotes longevity[J].Nature Cell Biology,2010,11(1):1305-14.
[7]赵中辉.水产品贮藏中生物胺的变化及组胺形成机制的研究[D].青岛:中国海洋大学,2011.
[8]Silla Santos M H.Biogenic amines:their importance in foods[J].International Journal of Food Microbiology,1996,29(2-3):213-231.
[9]Ten B B,Damink C,Joosten H M,et al.Occurrence and formation of biologically active amines in foods[J].International Journal of Food Microbiology,1990,11(1):73-84.
[10]Shalaby A R.Significance of biogenic amines to food safety and human health[J].Meat Research,2005,29(7):675-690.
[11]Hwang B S,Wang J T,Choong Y M.A rapid gas chromatographic method for the determination of histamine in fish and fish products[J].Food Chemistry,2003,82(2):329-334.
[12]马宝龙,屈旭斌.高效液相色谱法测定枸杞叶中精胺和亚精胺[J].宁夏工程技术,2011,10(1):48-50.
[13]AnetaJastrz?bska,Piasta A,Edward Szlyk.Application of ion chromatography for the determination of biogenic amines in food samples[J].Journal of Analytical Chemistry,2015,70(9):1131-1138.
[14]李燕君.薄层色谱法检测黄酒生物胺的研究[J].广州化学,2017,42(4):18-25.
[15]唐晗,王晓朋,吴中波,等.化学发光生物传感器检测食品中生物胺总量[J].食品安全质量检测学报,2014(5):1349-1356.
[16]杨姗姗,杨亚楠,李雪霖,等.在线固相萃取-毛细管高效液相色谱联用测定奶酪中的生物胺[J].分析化学,2016(3):396-402.
[17]Annesley T M.Ion suppression in mass spectrometry[J].Clinical Chemistry,2003,49(7):1041-1044.
[18]Matuszewski B K,Constanzer M L,Chavez-Eng C M.Matrix effect in quantitative LC/MS/MS analyses of biological fluids:a method for determination of finasteride in human plasma at picogram per milliliter concentrations[J].Analytical Chemistry,1998,70(5):882-889.
[19]González O,Blanco M E,Iriarte G,et al.Bioanalytical chromatographic method validation according to current regulations,with a special focus on the non-well defined parameters limit of quantification,robustness and matrix effect[J].Journal of Chromatography A,2014,1353:10-27.
[2]Jose Maria Landete,Rosario Munoz.Characterization of a second ornithine decarboxylase isolated from Morganella morganii[J].Journal of Food Protection,2008,71(3):657.
[3]Kalac P.Health effects and occurrence of dietary polyamines:a review for the period 2005-mid 2013[J].Food Chemistry,2014,161(11):27-39.
[4]Madeo F,Eisenberg T,Pietrocola F,et al.Spermidine in health and disease[J].Science,2018,359(6374):2788.
[5]Morselli E,Mariňo G,Bennetzen M V,et al.Spermidine and resveratrol induce autophagy by distinct pathways converging on the acetylproteome[J].Journal of Cell Biology,2011,192(6):615-629.
[6]Eisenberg T,Knauer H,Schauer A,et al.Induction of autophagy by spermidine promotes longevity[J].Nature Cell Biology,2010,11(1):1305-14.
[7]赵中辉.水产品贮藏中生物胺的变化及组胺形成机制的研究[D].青岛:中国海洋大学,2011.
[8]Silla Santos M H.Biogenic amines:their importance in foods[J].International Journal of Food Microbiology,1996,29(2-3):213-231.
[9]Ten B B,Damink C,Joosten H M,et al.Occurrence and formation of biologically active amines in foods[J].International Journal of Food Microbiology,1990,11(1):73-84.
[10]Shalaby A R.Significance of biogenic amines to food safety and human health[J].Meat Research,2005,29(7):675-690.
[11]Hwang B S,Wang J T,Choong Y M.A rapid gas chromatographic method for the determination of histamine in fish and fish products[J].Food Chemistry,2003,82(2):329-334.
[12]马宝龙,屈旭斌.高效液相色谱法测定枸杞叶中精胺和亚精胺[J].宁夏工程技术,2011,10(1):48-50.
[13]AnetaJastrz?bska,Piasta A,Edward Szlyk.Application of ion chromatography for the determination of biogenic amines in food samples[J].Journal of Analytical Chemistry,2015,70(9):1131-1138.
[14]李燕君.薄层色谱法检测黄酒生物胺的研究[J].广州化学,2017,42(4):18-25.
[15]唐晗,王晓朋,吴中波,等.化学发光生物传感器检测食品中生物胺总量[J].食品安全质量检测学报,2014(5):1349-1356.
[16]杨姗姗,杨亚楠,李雪霖,等.在线固相萃取-毛细管高效液相色谱联用测定奶酪中的生物胺[J].分析化学,2016(3):396-402.
[17]Annesley T M.Ion suppression in mass spectrometry[J].Clinical Chemistry,2003,49(7):1041-1044.
[18]Matuszewski B K,Constanzer M L,Chavez-Eng C M.Matrix effect in quantitative LC/MS/MS analyses of biological fluids:a method for determination of finasteride in human plasma at picogram per milliliter concentrations[J].Analytical Chemistry,1998,70(5):882-889.
[19]González O,Blanco M E,Iriarte G,et al.Bioanalytical chromatographic method validation according to current regulations,with a special focus on the non-well defined parameters limit of quantification,robustness and matrix effect[J].Journal of Chromatography A,2014,1353:10-27.