顶空气相色谱法测定白酒中氰化物含量
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摘要
目的建立顶空气相色谱法测定白酒中氰化物含量检测的方法,探究GB5009.36-2016第二法在白酒、白兰地、威士忌、朗姆酒等酒样中应用的区别。方法将酒样进碱解前处理后,以顶空进样器注入气相色谱仪进行分离,电子捕获检测器进行检测。以加标回收率为指标,对方法及前处理进行评价。结果国标第一法与第二法结果有较大的差别,碱解前处理的气相色谱法与国标第一法结果相近。用GB 5009.36-2016第二法测定白酒、白兰地、威士忌、朗姆酒等中的氰化物含量时,均无法得到较好的加标回收率;用GB5009.36-2016第二法检测伏特加、以食用酒精为酒基的露酒中的氰化物含量时可以得到较好的回收率。顶空气相色谱法测定白酒中氰化物含量时,线性相关系数r为0.9999,相对标准偏差(relative standard deviation,RSD)为8.0%,回收率为78.0%～1112.5%。结论顶空气相色谱法测定白酒中氰化物含量时能够得到与国标第一法相近的结果,该方法操简单、灵敏度高,结果准确度高,适合白酒中氰化物含量的测定。
Objective To establish a method for the determination of cyanide content in liquor by headspace gas chromatography,and to explore the difference between the application of GB 5009.36-2016 second method in liquors such as liquor,brandy,whiskey and rum.Methods After the wine sample was subjected to alkaline hydrolysis treatment,it was separated into a gas chromatograph by a headspace sampler,and an electron capture detector was used for detection.The method and pretreatment were evaluated by the spiked recovery rates.Results The results of the first method of the national standard and the second method were quite different.The gas chromatography with alkaline hydrolysis treatmentwas similar to the first method of the national standard.When the cyanide contents in white wine,brandy,whiskey,rum,etc.were determined by the second method of GB 5009.36-2016,no good spike recovery rate could be obtained.A better recovery rate could be obtained by detecting the cyanide content of vodka and the alcohol-based wine bythe second method of GB 5009.36-2016.When the cyanide contents in liquor were determined by headspace gas chromatography,the linear correlation coefficient r was 0.9999,the relative standard deviation(RSD) was 8.0%,and the recoveries were 78.0%-112.5%.Conclusion When the headspace gas chromatography method is used to determine the cyanide content in liquor,the results similar to the first method of the national standard can be obtained.The method is simple in operation,high in sensitivity and high in accuracy,which is suitable for the determination of cyanide content in liquor.
Objective To establish a method for the determination of cyanide content in liquor by headspace gas chromatography,and to explore the difference between the application of GB 5009.36-2016 second method in liquors such as liquor,brandy,whiskey and rum.Methods After the wine sample was subjected to alkaline hydrolysis treatment,it was separated into a gas chromatograph by a headspace sampler,and an electron capture detector was used for detection.The method and pretreatment were evaluated by the spiked recovery rates.Results The results of the first method of the national standard and the second method were quite different.The gas chromatography with alkaline hydrolysis treatmentwas similar to the first method of the national standard.When the cyanide contents in white wine,brandy,whiskey,rum,etc.were determined by the second method of GB 5009.36-2016,no good spike recovery rate could be obtained.A better recovery rate could be obtained by detecting the cyanide content of vodka and the alcohol-based wine bythe second method of GB 5009.36-2016.When the cyanide contents in liquor were determined by headspace gas chromatography,the linear correlation coefficient r was 0.9999,the relative standard deviation(RSD) was 8.0%,and the recoveries were 78.0%-112.5%.Conclusion When the headspace gas chromatography method is used to determine the cyanide content in liquor,the results similar to the first method of the national standard can be obtained.The method is simple in operation,high in sensitivity and high in accuracy,which is suitable for the determination of cyanide content in liquor.
引文
[1]郭忠,张文德.食品中的氰化物来源及其安全性的研究进展[J].中国食品卫生杂志,2014,26(4):404-408.Guo Z,Zhang WD.Research progress on source and safety of cyanide in food[J].Chin J Food Hyg,2014,26(4):404-408.
[2]王欢,张义明,彭小东,等.白酒中氰化物的研究进展[J].酿酒科技,2017,(8):112-115.Wang H,Zhang YM,Peng XD,et al.Research progress on cyanide in liquor[J].Liq-Mak Sci Technol,2017,(8):112-115.
[3]李源栋,樊林,钱海燕,等.酒中氰化物测定方法的研究进展[J].酿酒,2009,36(6):16-19.Li YD,Fan L,Qian HY,et al.Research advance of cyanide determination methods for wine[J].Liq-Mak,2009,36(6):16-19.
[4]GB 2757-2012食品安全国家标准蒸馏酒及其配制酒[S].GB 2757-2012 National food safety standard-Distilled spirits and their preparation liquor[S].
[5]国家食品药品监督管理总局.总局关于9批次食品不合格情况的通告[EB/OL].[2017-4-21].http://www.hebfda.gov.cn/CL0373/60421.html Circular of the state food and drug administration on 9 batches of unqualified food[EB/OL].[2017-4-21].http://www.hebfda.gov.cn/CL0373/60421.html
[6]四川省食品药品监督管理局.食品安全监督抽检信息公告[EB/OL].[2017-3-16].http://www.scfda.gov.cn/CL3336/123358.html Sichuan food and drug administration.Announcement of sampling inspection information of food safety supervision[EB/OL].[2017-3-16].http://www.scfda.gov.cn/CL3336/123358.html
[7]重庆市食品药品监督管理局.关于11批次食品不合格情况的通告[EB/OL].[2016-9-19].http://www.baipin.org/index/infodetail/id/2574Chongqing food and drug administration.Circular on 11 batches of unqualified food[EB/OL].[2016-9-19].http://www.baipin.org/index/infodetail/id/2574
[8]国家食品药品监督管理总局.总局关于42批次白酒不合格的通告[EB/OL].[2016-3-17].http://www.xinhuanet.com//politics/2016-03/17/c_128809058.htm China food and drug administration.Notice of 42 batches of liquor unqualified[EB/OL].[2016-3-17].http://www.xinhuanet.com//politics/2016-03/17/c_128809058.htm
[9]刘芯韵,张坤,易啸,等.离子色谱法测定蒸馏酒中氰化物含量的方法性能分析[J].食品与发酵科技,2017,53(2):94-95,126.Liu XY,Zhang K,Yi X,et al.Method performance analysis of determination of cyanide in distilled wines by ion chromatography[J].Food Ferment Sci Technol,2017,53(2):94-95,126.
[10]李悦,何颖,李彦懿,等.紫外-可见分光光度法测定3种酒中氰化物的浓度[J].酿酒科技,2017,(8):128-131.Li Y,He Y,Li YY,et al.Determination of cyanides concentration in 3kinds of alcoholic drinks by UV-Vis spectrophotometry[J].Liq-Mak Sci Technol,2017,(8):128-131.
[11]杜利君,刘晓林,高媛惠,等.顶空气相色谱法快速测定酒中氰化物含量[J].食品研究与开发,2017,38(11):131-133.Du LJ,Liu XY,Gao YH,et al.Determination of cyanide in wine by headspace gas chromatography[J].Food Res Dev,2017,38(11):131-133.
[12]Chinaka S,Takayama N,Michigami Y,et al.Simultaneous determination of cyanide and thiocyanate in blood by ion chromatography with fluorescence and ultraviolet detection[J].J Chromatogr B,1998,713(2):353-359.
[13]阎冠洲,钟其顶,李国辉,等.顶空气相色谱测定白酒中氰化物方法研究[J].酿酒科技,2013,(3):89-92.Yan GZ,Zhong QD,Li GH,et al.Study on the determination of cyanide content in liquor by headspace gas chromatography[J].Liq-Mak Sci Technol,2013,(3):89-92.
[14]方诚,凌芳,郑琦,等.异烟酸-吡唑啉酮光度法测定硫酸铵中氰化物[J].化学试剂,2017,39(11):1193-1195,1200.Fang C,Ling F,Zheng Q,et al.Isonicotinic acid-pyrazolone spectrophotometric determination of cyanide in ammonium sulfate[J].Chem Reag,2017,39(11):1193-1195,1200.
[15]张建,苏利进,李凯,等.GC-MS定性/HS-20顶空结合GC定量测定酒中痕量氰化物[J].酿酒科技,2014,(7):105-108.Zhang J,Su LJ,Li K,et al.GC-MS Qualitative/HS-20 headspace coupled with GC quantitative detection of trace cyanide content in liquor[J].Liq-Mak Sci Technol,2014,(7):105-108.
[16]GB 5009.36-2016食品安全国家标准食品中氰化物的测定[S].GB 5009.36-2016 National food safety standard-Determination of cyanide in food[S].
[2]王欢,张义明,彭小东,等.白酒中氰化物的研究进展[J].酿酒科技,2017,(8):112-115.Wang H,Zhang YM,Peng XD,et al.Research progress on cyanide in liquor[J].Liq-Mak Sci Technol,2017,(8):112-115.
[3]李源栋,樊林,钱海燕,等.酒中氰化物测定方法的研究进展[J].酿酒,2009,36(6):16-19.Li YD,Fan L,Qian HY,et al.Research advance of cyanide determination methods for wine[J].Liq-Mak,2009,36(6):16-19.
[4]GB 2757-2012食品安全国家标准蒸馏酒及其配制酒[S].GB 2757-2012 National food safety standard-Distilled spirits and their preparation liquor[S].
[5]国家食品药品监督管理总局.总局关于9批次食品不合格情况的通告[EB/OL].[2017-4-21].http://www.hebfda.gov.cn/CL0373/60421.html Circular of the state food and drug administration on 9 batches of unqualified food[EB/OL].[2017-4-21].http://www.hebfda.gov.cn/CL0373/60421.html
[6]四川省食品药品监督管理局.食品安全监督抽检信息公告[EB/OL].[2017-3-16].http://www.scfda.gov.cn/CL3336/123358.html Sichuan food and drug administration.Announcement of sampling inspection information of food safety supervision[EB/OL].[2017-3-16].http://www.scfda.gov.cn/CL3336/123358.html
[7]重庆市食品药品监督管理局.关于11批次食品不合格情况的通告[EB/OL].[2016-9-19].http://www.baipin.org/index/infodetail/id/2574Chongqing food and drug administration.Circular on 11 batches of unqualified food[EB/OL].[2016-9-19].http://www.baipin.org/index/infodetail/id/2574
[8]国家食品药品监督管理总局.总局关于42批次白酒不合格的通告[EB/OL].[2016-3-17].http://www.xinhuanet.com//politics/2016-03/17/c_128809058.htm China food and drug administration.Notice of 42 batches of liquor unqualified[EB/OL].[2016-3-17].http://www.xinhuanet.com//politics/2016-03/17/c_128809058.htm
[9]刘芯韵,张坤,易啸,等.离子色谱法测定蒸馏酒中氰化物含量的方法性能分析[J].食品与发酵科技,2017,53(2):94-95,126.Liu XY,Zhang K,Yi X,et al.Method performance analysis of determination of cyanide in distilled wines by ion chromatography[J].Food Ferment Sci Technol,2017,53(2):94-95,126.
[10]李悦,何颖,李彦懿,等.紫外-可见分光光度法测定3种酒中氰化物的浓度[J].酿酒科技,2017,(8):128-131.Li Y,He Y,Li YY,et al.Determination of cyanides concentration in 3kinds of alcoholic drinks by UV-Vis spectrophotometry[J].Liq-Mak Sci Technol,2017,(8):128-131.
[11]杜利君,刘晓林,高媛惠,等.顶空气相色谱法快速测定酒中氰化物含量[J].食品研究与开发,2017,38(11):131-133.Du LJ,Liu XY,Gao YH,et al.Determination of cyanide in wine by headspace gas chromatography[J].Food Res Dev,2017,38(11):131-133.
[12]Chinaka S,Takayama N,Michigami Y,et al.Simultaneous determination of cyanide and thiocyanate in blood by ion chromatography with fluorescence and ultraviolet detection[J].J Chromatogr B,1998,713(2):353-359.
[13]阎冠洲,钟其顶,李国辉,等.顶空气相色谱测定白酒中氰化物方法研究[J].酿酒科技,2013,(3):89-92.Yan GZ,Zhong QD,Li GH,et al.Study on the determination of cyanide content in liquor by headspace gas chromatography[J].Liq-Mak Sci Technol,2013,(3):89-92.
[14]方诚,凌芳,郑琦,等.异烟酸-吡唑啉酮光度法测定硫酸铵中氰化物[J].化学试剂,2017,39(11):1193-1195,1200.Fang C,Ling F,Zheng Q,et al.Isonicotinic acid-pyrazolone spectrophotometric determination of cyanide in ammonium sulfate[J].Chem Reag,2017,39(11):1193-1195,1200.
[15]张建,苏利进,李凯,等.GC-MS定性/HS-20顶空结合GC定量测定酒中痕量氰化物[J].酿酒科技,2014,(7):105-108.Zhang J,Su LJ,Li K,et al.GC-MS Qualitative/HS-20 headspace coupled with GC quantitative detection of trace cyanide content in liquor[J].Liq-Mak Sci Technol,2014,(7):105-108.
[16]GB 5009.36-2016食品安全国家标准食品中氰化物的测定[S].GB 5009.36-2016 National food safety standard-Determination of cyanide in food[S].