复方桔梗麻黄碱糖浆(Ⅱ)中防腐剂的检测
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摘要
目的:建立同时检测防腐剂苯甲酸、山梨酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯、脱氢乙酸的高效液相色谱法,并应用于复方桔梗麻黄碱糖浆(Ⅱ)中防腐剂的检测。方法:采用CAPCELL MGⅡC_(18)色谱柱(250 mm×4.6 mm,5μm)分离,以0.02 mol·L~(-1)醋酸铵溶液(冰醋酸调pH至4.0)为流动相A,甲醇为流动相B,梯度洗脱,流速为1.0 mL·min~(-1),检测波长为255 nm(苯甲酸、山梨酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯)、308 nm(脱氢乙酸)。结果:各化合物在相应的检测质量浓度范围内线性良好(r>0.999 6);精密度、稳定性试验的RSD<2.0%;平均回收率范围为98.3%~112.9%(n=9)。4家企业共43批样品均未检出山梨酸、对羟基苯甲酸酯类及脱氢乙酸;2家企业样品的苯甲酸含量与处方相符,另外2家的不相符。结论:本方法可用于复方桔梗麻黄碱糖浆(Ⅱ)中防腐剂的检测。
Objective:To establish an HPLC method for the simultaneous detection of preservatives(benzoic acid,sorbic acid,methylparaben,ethylparaben,propylparaben,butyl-p-hydroxybenzoate,dehydrogenation acid),and apply to the detection of preservation in compound Jiegeng Mahuangjian syrup(Ⅱ).Methods:SHISEIDO CAPCELL MG Ⅱ C18 column(250 mm×4.6 mm,5 μm)was adopted. The mobile phase consisted of 0.02 mol·L~(-1) ammonium acetate solution(using glacial acetic acid to adjust p H to 4)-methanol with gradient elution at the flow rate of 1.0 mL·min~(-1).The detective wavelength was 255 nm for benzoic acid,sorbic acid,methylparaben,ethylparaben,propylparaben,butyl-p-hydroxybenzoate and 308 nm for dehydrogenation acid.Results:The calibration curves of the above-mentioned components were linear in the range of the corresponding concentration.The RSDs of precision and stability test were less than 2.0%.The average recovery ranges were 98.3%~(-1)12.9%(n=9).No sorbic acid,parabens and dehydroacetic acid were detected in 43 batches of samples from 4 enterprises. The benzoic acid content of samples from 2 enterprises was consistent with the prescription and that from the other 2 was not.Conclusion:The method is suitable for the detection of preservative in compound Jiegeng Mahuangjian syrup(Ⅱ).
Objective:To establish an HPLC method for the simultaneous detection of preservatives(benzoic acid,sorbic acid,methylparaben,ethylparaben,propylparaben,butyl-p-hydroxybenzoate,dehydrogenation acid),and apply to the detection of preservation in compound Jiegeng Mahuangjian syrup(Ⅱ).Methods:SHISEIDO CAPCELL MG Ⅱ C18 column(250 mm×4.6 mm,5 μm)was adopted. The mobile phase consisted of 0.02 mol·L~(-1) ammonium acetate solution(using glacial acetic acid to adjust p H to 4)-methanol with gradient elution at the flow rate of 1.0 mL·min~(-1).The detective wavelength was 255 nm for benzoic acid,sorbic acid,methylparaben,ethylparaben,propylparaben,butyl-p-hydroxybenzoate and 308 nm for dehydrogenation acid.Results:The calibration curves of the above-mentioned components were linear in the range of the corresponding concentration.The RSDs of precision and stability test were less than 2.0%.The average recovery ranges were 98.3%~(-1)12.9%(n=9).No sorbic acid,parabens and dehydroacetic acid were detected in 43 batches of samples from 4 enterprises. The benzoic acid content of samples from 2 enterprises was consistent with the prescription and that from the other 2 was not.Conclusion:The method is suitable for the detection of preservative in compound Jiegeng Mahuangjian syrup(Ⅱ).
引文
[1]国家标准化管理委员会.GB/T 23377-2009食品中脱氢乙酸的测定高效液相色谱法[S].2009Standardization Administration of the People’s Republic of China.GB/T23377-2009 Determination of Dehydroacetic Acid in Food by High Performance Liquid Chromatography[S].2009
[2]国家标准化管理委员会.GB/T 5009.29-2003食品中山梨酸、苯甲酸的测定[S].2003Standardization Administration of the People’s Republic of China.GB/T 5009.29-2003 Determination of Sorbic Acid and Benzioc Acid in Foods[S].2003
[3]国家标准化管理委员会.GB 1886.31-2015食品添加剂对羟基苯甲酸乙酯[S].2015Standardization Administration of the People’s Republic of China.GB1886.31-2015 Food Additives Ethyl p-Hydroxybenzoate[S].2015
[4]国家标准化管理委员会.GB 5009.31-2016食品中对羟基苯甲酸脂类的测定[S].2016Standardization Administration of the People’s Republic of China.GB5009.31-2016 Determination of Benzoic Acid in Foods[S].2016
[5]国家质量监督检验检疫总局.SN/T 3545-2013出品食品中多种防腐剂的测定方法[S].2013AQSIQ.Determination of Various Preservatives in Foods for Export[S].2013
[6]国家卫生和计划生育委员会.GB 1886.183-2016食品添加剂苯甲酸[S].2016National Health and Family Planning Commission of the People’s Republic of China.Food Additives:Benzoic Acid[S].2016
[7]国家卫生和计划生育委员会.GB 1886.186-2016食品添加剂山梨酸[S].2016National Health and Family Planning Commission of the People’s Republic of China.Food Additives:Sorbic Acid[S].2016
[8]李丽莉,黄捷.HPLC法测定蛇胆川贝液中的防腐剂[J].中国实验方剂学杂志,2012,18(6):113LI LL,HUANG J.Determination of preservatives in Shedan Chuanbei mixture by HPLC[J].Chin J Exp Tradit Med Form,2012,18(6):113
[9]年四辉,李萍,刘丽华,等.HPLC法测定板蓝根及其制剂中水杨酸、苯甲酸的含量[J].中国实验方剂学杂志,2012,18(21):92NIAN SH,LI P,LIU LH,et al.Determination of salicylic acid and benzoic acid in Radix Isatidis and its preparations by HPLC[J].Chin J Exp Tradit Med Form,2012,18(21):92
[10]杨春林,李佳峻,胡强,等.高效液相色谱法同时测定饲料中多种酚类抗氧化剂和尼泊金酯类防腐剂[J].中国饲料,2013(1):39YANG CL,LI JJ,HU Q,et al.Simultaneous determination of phenolic antioxidants in feed and antimicrobial agents by HPLC[J].China Feed,2013(1):39
[11]尤妍,潘辉国,陈盼盼,等.高效液相色谱法同时测定饮料中5种添加剂[J].食品研究与开发,2016(4):164YOU Y,PAN HG,CHEN PP,et al.Determination of five additives in beverage by high performance liquid chromatography[J].Food Res Dev,2016(4):164
[12]迟秋池,陈燕,邵晓赟,等.高效液相色谱法同时测定可乐中苯甲酸、糖精钠、安赛蜜和咖啡因[J].食品安全质量检测学报,2016,7(2):617CHI QC,CHEN Y,SHAO XY,et al.Simultaneous determination of benzoic acid,sodium saccharin,acesulfame potassium and caffeine in cola soft drink by high performance liquid chromatography[J].J Food Saf Qual,2016,7(2):617
[13]陈晓红,赵永纲,姚珊珊,等.超快速液相色谱-串联质谱法测定黄酒和葡萄酒中的9种防腐剂和甜味剂[J].色谱,2011,29(12):1147CHEN XH,ZHAO YG,YAO SS,et al.Simultaneous determination of nine preservatives and sweeteners in yellow wine and wine by ultrafast liquid chromatography-tandem mass spectrometry[J].Chin J Chromatogr,2011,29(12):1147
[14]邵立君,王锡宁,王国玲,等.食品中脱氢乙酸检测方法的研究[J].食品科技,2014,39(4):292SHAO LJ,WANG XN,WANG GL,et al.Determination of dehydroacetic acid in food[J].Food Sci Technol,2014,39(4):292
[15]刘佟,王浩,苗雨田,等.高效液相色谱法同时测定食品中7种防腐剂[J].食品安全质量检测学报,2015,6(4):1148LIU T,WANG H,MIAO YT,et al.Determination of 7 preservatives in food using high performance liquid chromatography[J].J Food Saf Qual,2015,6(4):1148
[2]国家标准化管理委员会.GB/T 5009.29-2003食品中山梨酸、苯甲酸的测定[S].2003Standardization Administration of the People’s Republic of China.GB/T 5009.29-2003 Determination of Sorbic Acid and Benzioc Acid in Foods[S].2003
[3]国家标准化管理委员会.GB 1886.31-2015食品添加剂对羟基苯甲酸乙酯[S].2015Standardization Administration of the People’s Republic of China.GB1886.31-2015 Food Additives Ethyl p-Hydroxybenzoate[S].2015
[4]国家标准化管理委员会.GB 5009.31-2016食品中对羟基苯甲酸脂类的测定[S].2016Standardization Administration of the People’s Republic of China.GB5009.31-2016 Determination of Benzoic Acid in Foods[S].2016
[5]国家质量监督检验检疫总局.SN/T 3545-2013出品食品中多种防腐剂的测定方法[S].2013AQSIQ.Determination of Various Preservatives in Foods for Export[S].2013
[6]国家卫生和计划生育委员会.GB 1886.183-2016食品添加剂苯甲酸[S].2016National Health and Family Planning Commission of the People’s Republic of China.Food Additives:Benzoic Acid[S].2016
[7]国家卫生和计划生育委员会.GB 1886.186-2016食品添加剂山梨酸[S].2016National Health and Family Planning Commission of the People’s Republic of China.Food Additives:Sorbic Acid[S].2016
[8]李丽莉,黄捷.HPLC法测定蛇胆川贝液中的防腐剂[J].中国实验方剂学杂志,2012,18(6):113LI LL,HUANG J.Determination of preservatives in Shedan Chuanbei mixture by HPLC[J].Chin J Exp Tradit Med Form,2012,18(6):113
[9]年四辉,李萍,刘丽华,等.HPLC法测定板蓝根及其制剂中水杨酸、苯甲酸的含量[J].中国实验方剂学杂志,2012,18(21):92NIAN SH,LI P,LIU LH,et al.Determination of salicylic acid and benzoic acid in Radix Isatidis and its preparations by HPLC[J].Chin J Exp Tradit Med Form,2012,18(21):92
[10]杨春林,李佳峻,胡强,等.高效液相色谱法同时测定饲料中多种酚类抗氧化剂和尼泊金酯类防腐剂[J].中国饲料,2013(1):39YANG CL,LI JJ,HU Q,et al.Simultaneous determination of phenolic antioxidants in feed and antimicrobial agents by HPLC[J].China Feed,2013(1):39
[11]尤妍,潘辉国,陈盼盼,等.高效液相色谱法同时测定饮料中5种添加剂[J].食品研究与开发,2016(4):164YOU Y,PAN HG,CHEN PP,et al.Determination of five additives in beverage by high performance liquid chromatography[J].Food Res Dev,2016(4):164
[12]迟秋池,陈燕,邵晓赟,等.高效液相色谱法同时测定可乐中苯甲酸、糖精钠、安赛蜜和咖啡因[J].食品安全质量检测学报,2016,7(2):617CHI QC,CHEN Y,SHAO XY,et al.Simultaneous determination of benzoic acid,sodium saccharin,acesulfame potassium and caffeine in cola soft drink by high performance liquid chromatography[J].J Food Saf Qual,2016,7(2):617
[13]陈晓红,赵永纲,姚珊珊,等.超快速液相色谱-串联质谱法测定黄酒和葡萄酒中的9种防腐剂和甜味剂[J].色谱,2011,29(12):1147CHEN XH,ZHAO YG,YAO SS,et al.Simultaneous determination of nine preservatives and sweeteners in yellow wine and wine by ultrafast liquid chromatography-tandem mass spectrometry[J].Chin J Chromatogr,2011,29(12):1147
[14]邵立君,王锡宁,王国玲,等.食品中脱氢乙酸检测方法的研究[J].食品科技,2014,39(4):292SHAO LJ,WANG XN,WANG GL,et al.Determination of dehydroacetic acid in food[J].Food Sci Technol,2014,39(4):292
[15]刘佟,王浩,苗雨田,等.高效液相色谱法同时测定食品中7种防腐剂[J].食品安全质量检测学报,2015,6(4):1148LIU T,WANG H,MIAO YT,et al.Determination of 7 preservatives in food using high performance liquid chromatography[J].J Food Saf Qual,2015,6(4):1148