LILIC-Q/TOF对乳粉中羟脯氨酸的确证分析
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摘要
建立亲水作用色谱-四极杆飞行时间质谱测定乳粉中羟脯氨酸的确证方法。乳粉样品经盐酸水解后,以HLB固相萃取柱净化,经亲水作用色谱柱分离后,使用超高效液相色谱-四极杆/飞行时间质谱分别进行全扫描和羟脯氨酸的二级质谱扫描分析,以羟脯氨酸的色谱保留时间、母离子和碎片离子的精确质量数对其进行确证分析。方法的检测限优于0.1 mg/kg,可满足乳粉中非法添加羟脯氨酸的确证分析要求。
A confirmatory analytical method was developed for the determination of hydroxyproline in milk powder using hydrophilic interaction chromatography coupled with quadrupole-time of flight-mass spectrometry(HILIC-Q/TOF).The samples were hydrolyzed with hydrochloric acid,and cleaned up by solid phase extraction,and the protein was precipitated with acetonitrile subsequently. After separated on an Acquity UPLC BEH HILIC column,hydroxyproline was carried out in the full scan and daughter ion scan mode. The hydroxyproline was confirmed by the retention time,accurate mass of parent ion and fragment ions,and the detection limit was better than 0.1 mg/kg. The method was suitable for the confirmation of hydroxyproline in milk powder.
A confirmatory analytical method was developed for the determination of hydroxyproline in milk powder using hydrophilic interaction chromatography coupled with quadrupole-time of flight-mass spectrometry(HILIC-Q/TOF).The samples were hydrolyzed with hydrochloric acid,and cleaned up by solid phase extraction,and the protein was precipitated with acetonitrile subsequently. After separated on an Acquity UPLC BEH HILIC column,hydroxyproline was carried out in the full scan and daughter ion scan mode. The hydroxyproline was confirmed by the retention time,accurate mass of parent ion and fragment ions,and the detection limit was better than 0.1 mg/kg. The method was suitable for the confirmation of hydroxyproline in milk powder.
引文
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[20]赵善贞,邓晓军,彭涛,等.亲水性相互作用色谱-四极杆串联线性离子阱质谱测定蛋白食品中L-羟脯氨酸残留[J].分析化学,2011(9):1373-1379
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[22]冯志强,许银叶,黄永连,等.氨基酸自动分析仪测定胶原蛋白保健品中羟脯氨酸的含量[J].食品工业,2014,35(5):248-250
[23]蔡梅,吉文亮,刘华良,等.氨基酸自动分析仪对牛乳中羟脯氨酸快速测定方法研究[J].中国食品卫生杂志,2012,24(6):542-545
[24]曾暖茜,王洪健,周兴起,等.氨基酸自动分析仪对乳制品中羟脯氨酸的测定方法研究[J].现代食品科技,2008,24(7):719-721
[2]赵玉富,咸伟月.分光光度法测定乳及乳制品中L(-)-羟脯氨酸的改进研究[J].中国乳品工业,2013(10):36-37,46
[3]张强,赵富荣,邓小君.乳及乳制品中L(-)-羟脯氨酸测定方法的改进[J].现代科学仪器,2011(4):47-49
[4]彭亚锋,周耀斌,薛峰,等.比色法测定酱油中羟脯氨酸含量的探讨[J].中国调味品,2010,35(2):100-101
[5]罗凤莲,夏延斌,欧阳建勋,等,分光光度法测定鸡肉中的羟脯氨酸含量[J].食品科技,2010(1):122-124
[6]田艳玲,孙妍,陈婧,等.乳与乳制品中动物水解蛋白L-羟脯氨酸测定法[J].中国乳品工业,2009,37(6):49-50
[7]赵天珍,袁秀金,谭贵良,等.比色法快速测定奶粉和含乳饮料中游离L-羟脯氨酸[J].食品研究与开发,2008,29(12):111-113
[8]张俊杰,曾庆孝.比色法测定鱼鳞中羟脯氨酸的研究[J].食品科技,2004(4):83-85
[9]张怡评,易瑞灶,陈晖,等.离子色谱法测定鱼鳞胶原蛋白中羟脯氨酸含量方法的研究[J].中国海洋药物,2011,30(4):45-48
[10]俞斐,吴晖,陈延蕾.FMOC柱前衍生法测定鱼皮胶原肽中羟脯氨酸的含量[J].分析试验室,2016,35(2):220-223
[11]赵一晖,刘思洁,张培军,等.高效液相色谱法测定乳与乳制品中L-羟脯氨酸的含量[J].食品安全质量检测学报,2016,7(1):55-58
[12]赵秋莲,张丽宏,张秋梅,等.超高效液相色谱法测定原料乳中羟脯氨酸[J].中国畜牧兽医,2013,40(S1):85-88
[13]宫向红,刘慧慧,徐英江,等.DABS-Cl柱前衍生高效液相色谱法测定海参中羟脯氨酸含量[J].中国渔业质量与标准,2012,2(3):45-49
[14]王玮,张乔娜.鲜乳及乳粉中L-羟脯氨酸的柱前衍生高效液相色谱测定法[J].职业与健康,2012,28(16):1991-1993
[15]周桂友,侯艳芳,董新吉,等.对甲氧基苯磺酰氯柱前衍生测定尿中游离羟脯氨酸与脯氨酸[J].分析测试学报,2012,31(4):403-408
[16]黄会,宫向红,刘慧慧,等.柱前衍生高效液相色谱法测定水产品中羟脯氨酸含量[J].食品科学,2012(8):207-210
[17]于淑新,赵连海,王丰琳,等.高效液相色谱法测定奶粉中羟脯氨酸含量[J].分析仪器,2012(2):26-29
[18]蔡欣欣,张秀尧.液相色谱柱前衍生法测定乳及乳制品中羟脯氨酸[J].中国卫生检验杂志,2011(9):2147-2148
[19]黄蓓蓓.UPLC-MS/MS法测定乳品中L-羟脯氨酸的含量[J].食品研究与开发,2016,37(14):124-127
[20]赵善贞,邓晓军,彭涛,等.亲水性相互作用色谱-四极杆串联线性离子阱质谱测定蛋白食品中L-羟脯氨酸残留[J].分析化学,2011(9):1373-1379
[21]夏金根,陈波,姚守拙.高效液相色谱-质谱联用测定胶原蛋白中的羟脯氨酸[J].色谱,2008,26(5):595-598
[22]冯志强,许银叶,黄永连,等.氨基酸自动分析仪测定胶原蛋白保健品中羟脯氨酸的含量[J].食品工业,2014,35(5):248-250
[23]蔡梅,吉文亮,刘华良,等.氨基酸自动分析仪对牛乳中羟脯氨酸快速测定方法研究[J].中国食品卫生杂志,2012,24(6):542-545
[24]曾暖茜,王洪健,周兴起,等.氨基酸自动分析仪对乳制品中羟脯氨酸的测定方法研究[J].现代食品科技,2008,24(7):719-721