摘要
采用吹扫捕集气相色谱法建立了熏蒸剂氰和氰化氢在粮食(玉米、高粱、稻谷、小麦和大麦)中的分析方法,对粮食中氰和氰化氢预处理的吹扫温度、吹扫载气(N2)流量和吹扫时间等参数进行了优化,分析了吹扫捕集气相色谱测定的回收率、精密度、检出限和定量限等质量控制参数,并测定了实际熏蒸粮食中氰及其降解产物氰化氢残留量。结果表明,用50%磷酸溶液作溶剂,吹扫温度80℃、吹扫载气(N2)流量40 mL/min和吹扫时间90 min为最佳的吹扫方法参数。采用该方法测定粮食中氰和氰化氢的加标回收率分别为90.88%～96.25%和91.17%～95.83%,相对标准偏差(RSD)分别为0.36%～5.55%和0.90%～6.24%(n=6),检出限(LOD)分别为0.003 6 mg/kg和0.005 3 mg/kg(S/N=3),定量限(LOQ)分别为0.012 0 mg/kg和0.017 7mg/kg(S/N=10)。用吹扫捕集法检测熏蒸粮食中氰其降解产物氰化氢的残留量与溶剂顶空法测定结果相一致。
A method for the determination of cyanogen and hydrogen cyanide residues of fumigant in cereals, such as maize, sorghum, rice, wheat and barley, using gas chromatography with purge and trap was developed. Working parameters such as purge temperature ,current speed of carrier gas（ N2 ） and purge time for the purge of cyanogen and hydrogen cyanide in cereals were optimized using spiked lab blank samples. Quality control parameters such as recovery of standard, precision, limit of detection and limit of quantification for the process and residues of cyanogen and its degradation product - hydrogen cyanide in aged cereals were determined. Results showed that optimum conditions had purged for 90 min at 80℃ in the presence of 50% phosphoric acid solution as an acidifying reagent while purge velocity of carrier gas （ N2 ） was 40 mL/min. The recovery and accuracy of the method for monitoring of cyanogen and hydrogen cyanide in soil were 90.88% - 96.25% and 91.17% - 95.83% ,0.36% - 5.55% and 0.90% - 6.24% （n = 6 ）, respectively. The limit of detection （LOD） and limit of quantification （LOQ） of cyanogen and hydrogen cyanide were 0.0036 and 0.0053 mg/kg （ S/N = 3 ） ,0.0120 mg/kg and 0.0177 mg/kg （ S/N = 10）, respectively. The residues of cyanogen and its degradation product - hydrogen cyanide determined by this purge and trap method closely with those obtained by the solvent headspace method in aged cereals agreed
出处
《中国粮油学报》
EI
CAS
CSCD
北大核心
2013年第3期113-116,128,共5页
Journal of the Chinese Cereals and Oils Association
基金
国家自然科学基金(30960081)
江西省自然科学基金(20114BAB204010)
