气相色谱-质谱法测定白酒中塑化剂残留前处理方法的优化

Optimization of pretreatment method for determination of plasticizer residues in Chinese liquor by gas chromatography-mass spectrometry

中文关键词:  白酒  塑化剂  气相色谱-质谱法  乙醇含量  总酸  总酯  盐添加量

英文关键词:Chinese liquor  phthalates  gas chromatography-mass spectrometry  ethanol content  total acid  total ester  dosage of salt addition

中文摘要:

      目的 对气相色谱-质谱法(gas chromatography-mass spectrometer, GC-MS)检测白酒中17种塑化剂的前处理方法进行优化。方法 对试样中乙醇含量、总酸、总酯及盐添加量4个方面的变化进行了考察。用正己烷提取, 离心后取上清液进行分析, 根据回收结果筛选出最优的处理参数, 并通过对质控样的测定以验证其实际的检测效果。结果 当试样中的乙醇含量为10%(V/V)、盐添加量为0.3 g/mL时, 17种塑化剂的回收结果较为理想; 总酸含量在02.0 g/L及总酯含量在04.0 g/L范围内, 其浓度的变化对测定结果无显著影响。在0.101.00 μg/mL的浓度范围内, 17种塑化剂的检测响应值均具有良好的线性关系, 相关系数均大于0.99; 方法的检出限范围为0.020.06 mg/kg(n=10), 定量限范围为0.050.19 mg/kg(n=10); 当在空白样品中的加标量为0.10、0.50、1.00 mg/kg时, 17种塑化剂的平均回收率为80.0%120.0%, 相对标准偏差为2.47%6.97%(n=6); 采用本方法对含有14种塑化剂的质控样进行测定, 所有测定结果与指定值间的相对偏差均小于10%, 满足实际应用的精密度要求。结论 经前处理后的方法, 具有操作简易, 回收率高, 精密度好, 检测结果准确等优点, 可满足日常监督中对白酒塑化剂检测的需求。

英文摘要:

      Objective To optimize the pretreatment method of the gas chromatography-mass spectrometry (GC-MS) for detecting 17 phthalates in Chinese liquor. Methods Four parameters, the ethanol content, total acid, total ester and dosage of salt addition were investigated. The liquid supernatant was analyzed after extracting by n-hexane and centrifugation. According to the recovery rate results, the optimal parameters were obtained and verified by testing the quality control sample. Results The results showed that under the condition of 10%(V/V) ethanol content and 0.3 g/mL salt addition in liquor sample, the best recovery results of 17 phthalates could be acquired. The change of concentration in total acid in the concentration range of 02.0 g/L and total ester in the range of 04.0 g/L had no significant effect for the test results. The linear relations of 17 phthalates were good with all linear correlation and coefficients greater than 0.99 in the range of 0.101.00 μg/mL. The detection limit was 0.020.06 mg/kg (n=10) and the quantification limit was 0.050.19 mg/kg(n=10). When the addition standard concentration was 0.10, 0.50 and 1.00 mg/kg, the average recovery of 17 phthalates was 80.0%120.0%, and the relative standard deviation(RSD) was between 2.47%6.97%(n=6). The liquor quality control samples containing 14 phthalates were tested by this method and the relative deviation between all the measured results and the specified value was less than 10%, showing the satisfied precision. Conclusion After optimization of pretreatment, the method has advantages with simply pretreatment, high recovery rate, good precision and accurate test results, which is able to satisfy the phthalates detection in Chinese liquor in daily supervision.