气相色谱-质谱法同时测定果蔬清洗剂中12种防腐剂和抗氧化剂
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摘要
建立了气相色谱-质谱同时检测果蔬清洗剂中12种防腐剂和抗氧化剂的方法。果蔬清洗剂样品先加入乙醇,经旋转蒸发除去样品中的水分,然后用正己烷饱和的乙腈溶液提取,饱和氯化钠溶液洗涤净化,净化后的样品溶液浓缩后用乙腈定容。被测组分经HP-5MS UI石英毛细管色谱柱(30 m×0. 25 mm×0. 25μm)分离后在选择离子监测模式下测定。12种防腐剂和抗氧化剂在0. 1～10 mg/L范围内线性关系良好,相关系数(r2)>0. 999;检出限和定量限分别为0. 010～0. 030 mg/kg和0. 030～0. 090 mg/kg。按照建立的方法进行0. 2、2. 0和10 mg/kg 3个添加水平的加标回收试验,回收率为68. 3%～115. 3%,相对标准偏差为3. 1%～11. 3%。该法灵敏度高,定性准确,前处理净化效果好,适用于果蔬清洗剂中防腐剂和抗氧化剂的检测。
A method was established for the simultaneous determination of 12 preservatives and antioxidants in fruit and vegetable detergents by gas chromatography-mass spectrometry( GCMS). First,ethanol was added to remove the water in the sample by rotary evaporation and was extracted with acetonitrile in saturated n-hexane. Finally,the residual surfactant in the sample solution was removed with a saturated sodium chloride solution. The purified sample solution was concentrated and metered volume by acetonitrile. The preservatives and antioxidants were separated on a HP-5MS UI capillary column( 30 m×0. 25 mm×0. 25 μm),and detected in the selective ion monitoring( SIM) mode. The method had a good linearity in the range of 0. 1-10 mg/L with correlation coefficients( r 2) >0. 999,and the limits of detection( LODs) and limits of quantification( LOQs) were in the ranges of 0. 010-0. 030 mg/kg and 0. 030-0. 090mg/kg,respectively. The recoveries of the 12 preservatives and antioxidants at three spiked levels( 0. 2,2. 0 and 10 mg/kg) were 68. 3%-115. 3% with the relative standard deviations( RSDs) of 3. 1%-11. 3%.( n = 7) The method is sensitive and accurate,and can be suitable for the determination of preservatives and antioxidants in fruit and vegetable detergents.
A method was established for the simultaneous determination of 12 preservatives and antioxidants in fruit and vegetable detergents by gas chromatography-mass spectrometry( GCMS). First,ethanol was added to remove the water in the sample by rotary evaporation and was extracted with acetonitrile in saturated n-hexane. Finally,the residual surfactant in the sample solution was removed with a saturated sodium chloride solution. The purified sample solution was concentrated and metered volume by acetonitrile. The preservatives and antioxidants were separated on a HP-5MS UI capillary column( 30 m×0. 25 mm×0. 25 μm),and detected in the selective ion monitoring( SIM) mode. The method had a good linearity in the range of 0. 1-10 mg/L with correlation coefficients( r 2) >0. 999,and the limits of detection( LODs) and limits of quantification( LOQs) were in the ranges of 0. 010-0. 030 mg/kg and 0. 030-0. 090mg/kg,respectively. The recoveries of the 12 preservatives and antioxidants at three spiked levels( 0. 2,2. 0 and 10 mg/kg) were 68. 3%-115. 3% with the relative standard deviations( RSDs) of 3. 1%-11. 3%.( n = 7) The method is sensitive and accurate,and can be suitable for the determination of preservatives and antioxidants in fruit and vegetable detergents.
引文
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[3] GB/T 9985-2000
[4] GB/T 30795-2014
[5] Zhu H J,Zhang W Q,Yang Y W,et al. Chinese Journal of Chro m ato graphy,2014,32(1):95朱会卷,张卫强,杨艳伟,等.色谱,2014,32(1):95
[6] Fan S,Zou J H,Li L P,et al. Chinese Journal of Chromato graphy,2014,32(9):999范赛,邹建宏,李丽萍,等.色谱. 2014,32(9):999
[7] Zong W L. Science and Technology of Cereals,Oils and Fo o ds,2013,21(2):46宗万里.粮油食品科技,2013,21(2):46
[8] Lu J,Jiao X M,Tong X B,et al. China Surfactant Detergent&Co sm etics,2012,42(2):146陆军,矫筱蔓,佟晓波,等.日用化学工业,2012,42(2):146
[9] Hou R X,Wu Q. Chinese Journal of Health Laboratory Techno lo gy,2011,21(4):865侯瑞霞,吴青.中国卫生检验杂志,2011,21(4):865
[10] Wang Q. Fujian Analysis&Testing,2017,26(1):19王勍.福建分析测试,2017,26(1):19
[11] Lei T,Zhou Y B,Huang X R,et al. Physical Testing and Chem ical Analysis Part B:Chem ical Analysis,2010,46(12):1391雷涛,周耀斌,黄向荣,等.理化检验-化学分册,2010,46(12):1391
[12] Wang G X,Zhang L,Tang X J,et al. Physical Testing and Chem ical Analysis Part B:Chem ical Analysis,2015,51(1):35王改香,张磊,唐晓军,等.理化检验-化学分册,2015,51(1):35
[13] Wu T,Wang C,Wang X,et al. Chinese Journal of Analytical Chem istry,2007,35(10):1439武婷,王超,王星,等.分析化学. 2007,35(10):1439
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[16] Yang C L,Li J J,Hu Q,et al. China Feed,2013(1):39杨春林,李佳峻,胡强,等.中国饲料,2013(1):39
[17] Ling Y,Chu X G,Zhang F,et al. Chinese Journal of Chrom ato graphy,2011,29(8):723凌云,储晓刚,张峰,等.色谱,2011,29(8):723
[18] Zhang L,Kong X H,Li J H,et al. Chinese Journal of Analysis Labo rato ry,2014,33(1):43张璐,孔祥虹,李建华,等.分析试验室,2014,33(1):43
[19] Fu C Y,Liang Y,Xu W J,et al. Chinese Journal of Pharm aceutical Analysis,2016,36(8):1456符策奕,梁颖,许文佳,等.药物分析杂志,2016,36(8):1456
[20] Wang C Y,Li C F,Lin J F,et al. Chinese Journal of Chrom ato graphy,2017,35(5):509王成云,李成发,林君峰,等.色谱,2017,35(5):509
[21] Cao X Y. Guangdong Chemical Industry,2013,40(2):40曹晓瑶.广东化工,2013,40(2):40
[22] Wang P,Ma S Y,Guo L. Journal of Suihua University,2013,33(2):154王鹏,马松艳,郭丽.绥化学院报,2013,33(2):154
[23] Gao F Y,Zhang W B,Guan Y F,et al. Science China Chem istry,2014,44(7):1181高方圆,张维冰,关亚风,等.中国科学化学,2014,44(7):1181