顶空气相色谱-质谱法测定白酒中的氰化物含量
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摘要
目的建立顶空气相色谱-质谱法测定白酒中的氰化物含量的方法。方法优化顶空平衡温度、时间、pH值、氯胺T加入量,以顶空进样器注入气相色谱质谱联用仪进行分离检测,并应用该方法对市售的米香型、清香型、豉香型和浓香型4种香型的白酒进行加标后检测。结果白酒中的氰化物在0.001～0.2 mg/L线性范围内线性关系良好,回归系数r~2=0.9996,检出限为0.01mg/L(S/N≥3),定量限为0.03mg/L(S/N≥10),加标回收率在71.6%～116.2%之间,相对标准偏差(relative standard deviation, RSD)为1.3%(n=6)。结论该方法简便快捷,结果准确度高,相比国标中的气相色谱法,明显缩短了检测周期,提高了检测效率,可用于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-mass spectrometry(GC-MS). Methods The headspace equilibrium temperature, time, pH value and the amount of chloramine T were optimized, and the samples were detected by GC-MS with headspace sampler.The method was applied to detect 4 kinds of liquor including rice-flavor, fen-flavor, soybean-flavor and luzhou flavor that adding cyanide standard solution. Results Cyanide content in liquor had good linear relationships in the range of 0.001-0.2 mg/L, and the correlation coefficient(r~2) was 0.9996. The limit of the detection was 0.01 mg/L(S/N≥3)and the limit of quantification was 0.03 mg/L(S/N≥10). The recoveries were 71.6%-116.2%, with the relative standard deviations of 1.3%(n=6). Conclusion This method is simple in operation and high in accuracy. Compared with the gas chromatography method in the national standard, this method obviously shortens the detection period and improves the detection efficiency, which can be used 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-mass spectrometry(GC-MS). Methods The headspace equilibrium temperature, time, pH value and the amount of chloramine T were optimized, and the samples were detected by GC-MS with headspace sampler.The method was applied to detect 4 kinds of liquor including rice-flavor, fen-flavor, soybean-flavor and luzhou flavor that adding cyanide standard solution. Results Cyanide content in liquor had good linear relationships in the range of 0.001-0.2 mg/L, and the correlation coefficient(r~2) was 0.9996. The limit of the detection was 0.01 mg/L(S/N≥3)and the limit of quantification was 0.03 mg/L(S/N≥10). The recoveries were 71.6%-116.2%, with the relative standard deviations of 1.3%(n=6). Conclusion This method is simple in operation and high in accuracy. Compared with the gas chromatography method in the national standard, this method obviously shortens the detection period and improves the detection efficiency, which can be used for the determination of cyanide content in liquor.
引文
[1]李悦,李彦懿,肖得力.氰化物定量检测方法应用研究进展[J].药物分析杂志,2016,36(12):2075-2083.Li Y,Li YY,Xiao DL.Progress in the application of cyanide quantitative detection[J].Chin J Pharm Anal,2016,36(12):2075-2083.
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[3]Abigale J,Curtis C,Charles G,et al.Simultaneous determination of cyanide and carbonyls in cyanogenic plants by gas chromatographyelectron capture/photoionization detection[J].Analyst,2002,127:1446-1449.
[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]李南,何海茵,郑悦珊,等.顶空气相色谱法测定白酒中氰化物含量[J].食品安全质量检测学报,2019,10(1):240-244.Li N,He HY,Zheng YS,et al.Determination of cyanide in liquor by headspace gas chromatography[J].J Food Saf Qual,2019,10(1):240-244.
[6]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].
[7]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 XL,Gao YH,et al.Determination of cyanide in wine by headspace gas chromatography[J].Food Res Dev,2017,38(11):131-133.
[8]邸玉敏,朱军,常靖,等.氰化物检测方法研究进展[J].理化检验(化学分册),2011,47(12):1491-1494.Qiu YM,Zhu J,Chan J,et al.Recent advance of detection method of cyanide[J].Phys Test Chem Anal B,2011,47(12):1491-1494.
[9]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].Liquor-Mak,2009,36(6):16-19.
[10]Scientific Opinion of the Panel on Contaminants.Ethyl carbamate and hydrocyanic acid in food and beverages[J].EFSA J,2007,551:1-44.
[11]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].Liquor-Mak Sci Technol,2017,(8):112-115.
[12]吴建军,薛民杰,朱力敏.顶空-气相色谱-质谱法测定富马酸二甲酯(DMF)胶囊中硫酸二甲酯(DMS)的定性、定量分析方法[J].广东化工,2017,44(20):163-164.Wu JJ,Xue MJ,Zhu LM.Qualitative and quantitative analysis of dimethyl sulfate(DMS)in dimethyl fumarate(DMF)capsule by headspace GC-MS[J].Guangdong Chem Ind,2017,44(20):163-164.
[13]时丽艳,赵娜,陈锐,等.顶空-气相色谱-质谱法测定环氧涂料中6种挥发性有机化合物[J].中国标准化,2018,(12):187-189.Shi LY,Zhao N,Chen Y,et al.Determination of 6 volatile organic compounds in epoxy coatings by headspace gas chromatography-mass spectrometry[J].Chin Standard,2018,(12):187-189.
[14]石玲玲,孙欣,陈章庭,等.顶空气相色谱-质谱法测定食用植物油中溶剂残留[J].检验检疫学刊,2018,28(1):1-4.Shi LL,Sun X,Chen ZT,et al.Determination of residual solvents inedible vegetable oils by HS-GC-MS[J].J Inspect Quarant,2018,28(1):1-4.
[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].Liquor-Mak Sci Technol,2014,(7):105-108.
[2]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].Liquor-Mak Sci Technol,2013,(3):89-92.
[3]Abigale J,Curtis C,Charles G,et al.Simultaneous determination of cyanide and carbonyls in cyanogenic plants by gas chromatographyelectron capture/photoionization detection[J].Analyst,2002,127:1446-1449.
[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]李南,何海茵,郑悦珊,等.顶空气相色谱法测定白酒中氰化物含量[J].食品安全质量检测学报,2019,10(1):240-244.Li N,He HY,Zheng YS,et al.Determination of cyanide in liquor by headspace gas chromatography[J].J Food Saf Qual,2019,10(1):240-244.
[6]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].
[7]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 XL,Gao YH,et al.Determination of cyanide in wine by headspace gas chromatography[J].Food Res Dev,2017,38(11):131-133.
[8]邸玉敏,朱军,常靖,等.氰化物检测方法研究进展[J].理化检验(化学分册),2011,47(12):1491-1494.Qiu YM,Zhu J,Chan J,et al.Recent advance of detection method of cyanide[J].Phys Test Chem Anal B,2011,47(12):1491-1494.
[9]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].Liquor-Mak,2009,36(6):16-19.
[10]Scientific Opinion of the Panel on Contaminants.Ethyl carbamate and hydrocyanic acid in food and beverages[J].EFSA J,2007,551:1-44.
[11]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].Liquor-Mak Sci Technol,2017,(8):112-115.
[12]吴建军,薛民杰,朱力敏.顶空-气相色谱-质谱法测定富马酸二甲酯(DMF)胶囊中硫酸二甲酯(DMS)的定性、定量分析方法[J].广东化工,2017,44(20):163-164.Wu JJ,Xue MJ,Zhu LM.Qualitative and quantitative analysis of dimethyl sulfate(DMS)in dimethyl fumarate(DMF)capsule by headspace GC-MS[J].Guangdong Chem Ind,2017,44(20):163-164.
[13]时丽艳,赵娜,陈锐,等.顶空-气相色谱-质谱法测定环氧涂料中6种挥发性有机化合物[J].中国标准化,2018,(12):187-189.Shi LY,Zhao N,Chen Y,et al.Determination of 6 volatile organic compounds in epoxy coatings by headspace gas chromatography-mass spectrometry[J].Chin Standard,2018,(12):187-189.
[14]石玲玲,孙欣,陈章庭,等.顶空气相色谱-质谱法测定食用植物油中溶剂残留[J].检验检疫学刊,2018,28(1):1-4.Shi LL,Sun X,Chen ZT,et al.Determination of residual solvents inedible vegetable oils by HS-GC-MS[J].J Inspect Quarant,2018,28(1):1-4.
[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].Liquor-Mak Sci Technol,2014,(7):105-108.