离子色谱-抑制电导法测定卷烟爆珠中挥发性脂肪酸
何鹏程,王东翔,郑秀瑾,张彬彬,胡立梅
1. 山东中烟工业有限责任公司青岛卷烟厂,山东青岛 266101; 2. 青岛盛瀚色谱技术有限公司,山东青岛 266101
Determination of volatile fatty acids in cigarette breakable capsules by ion chromatography suppressed conductivity method
HE Pengcheng1, WANG Dongxiang1, ZHENG Xiujin2, ZHANG Binbin2, HU Limei2
1. Qingdao Cigarette Factory, China Tobacco Shandong Industry Co., Ltd., Qingdao 266101, China; 2. Qingdao Shenghan Chromatogram Technology Co., Ltd., Qingdao 266101, China
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1 mL 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0.22 μm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0.8764~10.23 μg/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。
Abstract: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-C18 pretreatment column and 0.22 μm 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 - 10.23 μg/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.
关键词:离子色谱法;卷烟爆珠;挥发性脂肪酸
Keywords:ion chromatography; cigratte breakable capsules; volatile fatty acid
本文引用格式:
何鹏程,王东翔,郑秀瑾,等.离子色谱-抑制电导法测定卷烟爆珠中挥发性脂肪酸[J].化学分析计量,2023,32(4):35.
HE Pengcheng,WANG Dongxiang,ZHENG Xiujin,et al. Determination of volatile fatty acids in cigarette breakable capsules by ionchromatography suppressed conductivity method[J]. Chemical Analysis and Meterage,2023,32(4):35.
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