摘要
建立离子色谱法同时测定卷烟爆珠中甲酸、乙酸、丙酸、丁酸、戊酸、己酸的分析方法。500 mg样品用1mL 0.1 mol/L KOH溶液固定,压碎爆珠壁,用超纯水溶解,涡旋振荡提取,过SPE-C18柱和0.22μm滤膜后,以5 mmol/L KOH淋洗液等度洗脱,流量为1.0 mL/min,在柱温45℃条件下,经SH-AP-4型阴离子色谱柱分离,采用电导检测器检测,色谱峰面积外标法定量。6种脂肪酸在0.1~10 mg/L的质量浓度范围内与色谱峰面积线性关系良好,相关系数均大于0.999,方法检出限为0.876 4~10.23μg/L,测定结果的相对标准偏差为0.63%~3.00%(n=6),样品加标回收率为84.75%~115.4%。该方法可用于卷烟爆珠中挥发性脂肪酸的检测。
A method for simultaneous determination of formic acid,acetic acid,propionic acid,butyric acid,valeric acid and caproic acid in cigarette breakable capsules by ion chromatography was established.500 mg sample was fixed with 1 mL 0.1 mol/L KOH solution with the capsule wall curshed,dissolved with ultrapure water,extracted by vortexing,filtrated with SPE-C 18 pretreatment column and 0.22μm membrane.The filtrate was separated by SH-AP-4 anion column under the condition of isocratic elution of 5 mmol/L KOH with the flow rate of 1.0 mL/min at the column temperature of 45℃,the volatile fatty acids in the sample was determined by a conductivity detector,and quantified by external standard method.The mass concentration of six volatile fatty acids had a good linear relationship with the chromatographic peak areas in the range of 0.1-10 mg/L with the correlation coefficients all more than 0.999.The detection limits of the method were 0.8764-10.23μg/L,the relative standard deviations of the detection results were 0.63%-3.00%(n=6),and the recoveries were 84.75%-115.4%.This method is suitable for determination of volatile fatty acids in cigarette breakable capsules.
作者
何鹏程
王东翔
郑秀瑾
张彬彬
胡立梅
HE Pengcheng;WANG Dongxiang;ZHENG Xiujin;ZHANG Binbin;HU Limei(Qingdao Cigarette Factory,China Tobacco Shandong Industry Co.,Ltd.,Qingdao 266101,China;Qingdao Shenghan Chromatogram Technology Co.,Ltd.,Qingdao 266101,China)
出处
《化学分析计量》
CAS
2023年第4期35-39,68,共6页
Chemical Analysis And Meterage
关键词
离子色谱法
卷烟爆珠
挥发性脂肪酸
ion chromatography
cigratte breakable capsules
volatile fatty acid
