柱前衍生化-顶空-气相色谱法测定食品中双乙酸钠和丙酸盐的含量
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摘要
称取食品样品5.000 0g置于50mL容量瓶中,加入1.0g·L~(-1)丁酸标准溶液1mL作为内标,加水约25mL,涡旋混匀,超声提取30min,使双乙酸钠和丙酸钙从样品溶出进入溶液中,加水至刻度,摇匀,过滤,分取滤液5mL置于顶空瓶中,加入硫酸-甲醇(15+85)混合液2mL,盖紧瓶盖,在85℃进行衍生反应30min。然后在进样量为1mL的条件下,用DB-624色谱柱作为分离柱,在70～240℃区间按程序升温条件进行色谱分离,并用氢火焰离子化检测器(FID)进行检测。双乙酸钠和丙酸钙(以丙酸计)的线性范围均在200mg·L~(-1)以内。另测得上述2种化合物(丙酸钙以丙酸计)的检出限(3S/N)均为0.01g·kg~(-1)。取3种食品作为基质,加入分析物的标准溶液进行回收试验,测得回收率在95.1%～105%之间,测定值的相对标准偏差(n=6)≤5.0%。对3种食品样品各加相同量(0.50g·kg~(-1))的两种待测物标准溶液后,分别按试验方法和国家标准方法进行测定,所得2种方法的测定结果之间无显著差异。
5.000 0 g of food sample were placed into a 50 mL volumetric,and 1 mL of 1.0 g·L~(-1) butyric acid standard solution was added as internal standard.About 25 mL of water were added and the mixture was mixed vortically and extracted ultrasonically for 30 min to have the diacetate and propionate dissolved in water.After diluting to mark with water and mixing thoroughly,the mixture was filtered and 5 mL of the filtrate were transferred to the head-space flask.2 mL of the mixture of H_2SO_4 and methanol(15+85)were added and the HSflask was closed tightly with its cap.Derivatization was taken place in the HS-flask at 85℃for 30 min.An aliquot of 1 mL of the solution in HS-flask was introduced into and separated on the DB-624 chromatographic column under the programed temperature elevation condition in the interval from 70 ℃to 240 ℃.The analytes were determined by the H_2-FID.Linearity ranges of sodium diacetate and calcium propionate(expressed as propionic acid)were obtained in the same range within 200 mg·L~(-1).And values of detection limits(3 S/N)found for sodium diacetate and calcium propronate(expressed as propionic acid)were same as 0.01 g·kg~(-1).3 kinds of blank food samples were taken as matrixes,and tests for recovery and precision were made by standard addition method with 6 parallel determinations,giving values of recovery in the range of 95.1%to 105%,and values of RSDs(n=6)≤5.0%.On the base of the 3 food samples,same amounts(0.50 g·kg~(-1))of standard solutions of the 2 analytes were added,and the synthetic samples were analyzed by the present method and the method given in GB standards,giving results with good conformity and without significant deviation.
5.000 0 g of food sample were placed into a 50 mL volumetric,and 1 mL of 1.0 g·L~(-1) butyric acid standard solution was added as internal standard.About 25 mL of water were added and the mixture was mixed vortically and extracted ultrasonically for 30 min to have the diacetate and propionate dissolved in water.After diluting to mark with water and mixing thoroughly,the mixture was filtered and 5 mL of the filtrate were transferred to the head-space flask.2 mL of the mixture of H_2SO_4 and methanol(15+85)were added and the HSflask was closed tightly with its cap.Derivatization was taken place in the HS-flask at 85℃for 30 min.An aliquot of 1 mL of the solution in HS-flask was introduced into and separated on the DB-624 chromatographic column under the programed temperature elevation condition in the interval from 70 ℃to 240 ℃.The analytes were determined by the H_2-FID.Linearity ranges of sodium diacetate and calcium propionate(expressed as propionic acid)were obtained in the same range within 200 mg·L~(-1).And values of detection limits(3 S/N)found for sodium diacetate and calcium propronate(expressed as propionic acid)were same as 0.01 g·kg~(-1).3 kinds of blank food samples were taken as matrixes,and tests for recovery and precision were made by standard addition method with 6 parallel determinations,giving values of recovery in the range of 95.1%to 105%,and values of RSDs(n=6)≤5.0%.On the base of the 3 food samples,same amounts(0.50 g·kg~(-1))of standard solutions of the 2 analytes were added,and the synthetic samples were analyzed by the present method and the method given in GB standards,giving results with good conformity and without significant deviation.
引文
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[8]赖国银,林建忠,曾琪,等.凯氏定氮蒸馏装置-高效液相色谱法同时测定蚝油等食品中丙酸钠(钙)和双乙酸钠[J].食品科学,2017,38(4):270-274.
[9]林晶.顶空气相色谱法测定糕点中双乙酸钠和丙酸盐的含量[J].广东化工,2017,44(11):264-265.
[10]朱益雷,刘文霞,罗小妹,等.顶空气相色谱法测定保健酒及其原料中的甲酸[J].养生保健指南,2016(35):223-223.
[11]赵好,查河霞,赵士权.自动顶空-气相色谱法测定工作场所空气中甲酸和乙酸[J].理化检验-化学分册,2017,53(5):572-574.
[12]方道赠,隋玉杰,项林敏.化妆品中丙酸及其盐类检测方法的研究[J].广东化工,2016,43(18):77-78.
[13]张全美,王守卿,张彦.糕点食品中丙酸盐测定方法的改进[J].科技创新导报,2013,10(19):125-127.
[14] YANG M H,CHOONG Y M.A rapid gas chromatographic method for direct determination of shortchain(C2-C12)volatile organic acids in foods[J].Food Chemistry,2001,75(1):101-108.
[15]杨乙强.顶空进样-气相色谱法测定食品中丙酸盐[J].上海计量测试,2010,37(2):13-15.
[16]张思群,王志元,许毅.自动进样顶空气相色谱法连续测定食品中丙酸盐[J].食品科学,2002,23(11):104-106.
[17]张伟,李晓君,张静,等.柱前衍生-气相色谱法同时测定功能食品中8种有机酸[J].分析试验室,2014,2:175-179.
[18] DELBARRIO M A,HU J,ZHOU P Z,et al.Simultaneous determination of formic acid and formaldehyde in pharmaceutical excipients using headspace GC/MS[J].Journal of Pharmaceutical and Biomedical Analysis,2006,41(3):738-743.
[2]裴世春,张东杰,程远,等.用Budget方法评估食品防腐剂摄入量[J].粮油食品科技,2006,14(4):42-44.
[3]梁宝爱.食品中防腐剂丙酸钠、丙酸钙检测方法的研究[J].现代仪器,2009,15(4):34-36.
[4]卢兰香,孙珊珊,薛霞,等.高效液相色谱法测定食品中丙酸及其盐类[J].食品工业科技,2019,40(11):234-240.
[5] GB 5009.277-2016食品安全国家标准食品中双乙酸钠的测定[S].
[6] GB 5009.120-2016食品安全国家标准食品中丙酸钠、丙酸钙的测定[S].
[7]郝媛媛.高效液相色谱法同时测定食品中丙酸钙(钠)和双乙酸钠[J].化学分析计量,2016,25(6):59-61.
[8]赖国银,林建忠,曾琪,等.凯氏定氮蒸馏装置-高效液相色谱法同时测定蚝油等食品中丙酸钠(钙)和双乙酸钠[J].食品科学,2017,38(4):270-274.
[9]林晶.顶空气相色谱法测定糕点中双乙酸钠和丙酸盐的含量[J].广东化工,2017,44(11):264-265.
[10]朱益雷,刘文霞,罗小妹,等.顶空气相色谱法测定保健酒及其原料中的甲酸[J].养生保健指南,2016(35):223-223.
[11]赵好,查河霞,赵士权.自动顶空-气相色谱法测定工作场所空气中甲酸和乙酸[J].理化检验-化学分册,2017,53(5):572-574.
[12]方道赠,隋玉杰,项林敏.化妆品中丙酸及其盐类检测方法的研究[J].广东化工,2016,43(18):77-78.
[13]张全美,王守卿,张彦.糕点食品中丙酸盐测定方法的改进[J].科技创新导报,2013,10(19):125-127.
[14] YANG M H,CHOONG Y M.A rapid gas chromatographic method for direct determination of shortchain(C2-C12)volatile organic acids in foods[J].Food Chemistry,2001,75(1):101-108.
[15]杨乙强.顶空进样-气相色谱法测定食品中丙酸盐[J].上海计量测试,2010,37(2):13-15.
[16]张思群,王志元,许毅.自动进样顶空气相色谱法连续测定食品中丙酸盐[J].食品科学,2002,23(11):104-106.
[17]张伟,李晓君,张静,等.柱前衍生-气相色谱法同时测定功能食品中8种有机酸[J].分析试验室,2014,2:175-179.
[18] DELBARRIO M A,HU J,ZHOU P Z,et al.Simultaneous determination of formic acid and formaldehyde in pharmaceutical excipients using headspace GC/MS[J].Journal of Pharmaceutical and Biomedical Analysis,2006,41(3):738-743.