An ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-MS/MS) method was developed and optimized for the simultaneous determination of 36 preservatives in protein drinks and liquid condiments by the pretreatment method of combining extraction and purification. The samples were purified with saturated sodium chloride solution (adjusting pH to 3 with phosphoric acid) and extracted with acetonitrile-methanol (9∶1, volume ratio) (containing 0.2% formic acid). The analytes were separated on a C18 chromatographic column using gradient elution with methanol-5 mmol/L ammonium acetate as the mobile phase, detected by MS/MS in both positive ion and negative ion mode using dynamic multiple reaction monitoring, and finally quantified by the matrix-matched external standard method. Results showed that good linearity was observed for the 36 compounds with correlation coefficients≥0.999 in the concentration range of 1-250 ng/mL, and the limits of quantitation were between 0.04 mg/kg and 0.2 mg/kg. The average recoveries of blank samples were in the range of 75%-119%, with relative standard deviations of 0.90%-9.8%. The established high-throughput detection method is sensitive, rapid, accurate, and simple, can effectively reduce matrix interference, reduce detection cost, shorten the detection cycle, and greatly improve the qualitative and quantitative detection efficiency of various preservatives.
[1] 王建文. “食以味为先” 调味品齐走 “高端路”[J].中国盐业, 2017(13):78-79.
WANG J W.“taste first” and “high-end road” for condiments[J].China Salt Industry, 2017(13):78-79.
[2] 陈静, 毛北萍, 郑荣, 等.高效液相色谱-质谱联用法同时测定8种不同基质类型化妆品中的23种防腐剂[J].日用化学工业, 2018, 48(12):717-724.
CHEN J, MAO B P, ZHENG R, et al.Simultaneous determination of 23 preservatives in 8 different matrixes of cosmetics by HPLC-MS/MS[J].China Surfactant Detergent & Cosmetics, 2018, 48(12):717-724.
[3] 吴思湟, 姜巧, 陈翘, 等.尼泊金丁酯用于24 h尿液标本生化项目测定的研究[J].检验医学与临床, 2018, 15(22):3345-3348.
WU S H, JIANG Q, CHEN Q, et al.The effects of butylparaben used as a preservative on the biochemical determination of 24-hour urine specimen[J].Laboratory Medicine and Clinic, 2018, 15(22):3345-3348.
[4] 王骏, 胡梅, 张卉, 等.超高效液相色谱快速测定饮料中的16种食品添加剂[J].食品科学, 2010, 31(2):195-198.
WANG J, HU M, ZHANG H, et al.Rapid determination of sixteen kinds of food additives in beverages by ultra performance liquid chromatography[J].Food Science, 2010, 31(2):195-198.
[5] 汪辉, 曹小彦, 李林, 等.反相高效液相色谱法对果蔬汁饮料中14种常见食品添加剂的快速测定[J].分析测试学报, 2009, 28(10):1194-1197.
WANG H, CAO X Y, LI L, et al.Determination of fourteen familiar food additives in fruit and vegetable drink by fast reversed-phase high performance liquid chromatography[J].Journal of Instrumental Analysis, 2009, 28(10):1194-1197.
[6] 凌云, 储晓刚, 张峰, 等.超高效液相色谱-串联质谱法同时测定调味料中的17种防腐剂和抗氧化剂[J].色谱, 2011, 29(8):723-730.
LING Y, CHU X G, ZHANG F, et al.Simultaneous determination of 17 preservatives and antioxidants in condiments using ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry[J].Chinese Journal of Chromatography, 2011, 29(8):723-730.
[7] 马传江. 高效液相色谱-串联质谱法测定中药口服液中23种防腐剂[J].药物分析杂志, 2019, 39(9):1651-1659.
MA C J.Simultaneous determination of 23 preservatives in traditional Chinese medicine oral liquid by liquid chromatography tandem mass spectrometry[J].Chinese Journal of Pharmaceutical Analysis, 2019, 39(9):1651-1659.
[8] 邢海艳, 孙丽, 吴旭, 等.高效液相色谱法同时测定化妆品中9种4-羟基苯甲酸酯类防腐剂[J].化学分析计量, 2021, 30(5):46-50.
XING H Y, SUN L, WU X, et al.Simultaneous determination of nine kinds of 4-hydroxybenzoate preservatives in cosmetics by high performance liquid chromatography[J].Chemical Analysis and Meterage, 2021, 30(5):46-50.
[9] 符策奕, 梁颖, 许文佳, 等.液相色谱串联质谱法同时测定6类不同剂型化妆品中10种防腐剂[J].药物分析杂志, 2016, 36(8):1456-1464.
FU C Y, LIANG Y, XU W J, et al.Simultaneous determination of 10 preservatives in 6 different dosage forms of cosmetics by HPLC-MS/MS[J].Chinese Journal of Pharmaceutical Analysis, 2016, 36(8):1456-1464.
[10] 郑荣, 茹歌, 王柯.高效液相色谱-串联质谱法测定化妆品中16种防腐剂[J].中国卫生检验杂志, 2016, 26(19):2758-2761.
ZHENG R, RU G, WANG K.Simultaneous determination of 16 preservatives in cosmetics by liquid chromatography tandem mass spectrometry[J].Chinese Journal of Health Laboratory Technology, 2016, 26(19):2758-2761.
[11] 汤丽昌, 陈高健, 梁国华.超高效液相色谱-串联质谱法同时测定食醋、酱油及料酒中的13种甜味剂和防腐剂[J].食品安全质量检测学报, 2021, 12(6):2181-2188.
TANG L C, CHEN G J, LIANG G H.Simultaneous determination of 13 preservatives and sweeteners in vinegar, soy sauce and seasoning wine by ultra performance liquid chromatography-tandem mass spectrometry[J].Journal of Food Safety & Quality, 2021, 12(6):2181-2188.
[12] 向君毅, 曾小平, 陈振雄.高通量同时测定食品中多种防腐剂、甜味剂、着色剂及抗氧化剂的检测技术研究[J].科技与创新, 2018(10):94-95.
XIANG J Y, ZENG X P, CHEN Z X.Study on high-throughput simultaneous determination of preservatives, sweeteners, colorants and antioxidants in food[J].Science and Technology & Innovation, 2018(10):94-95.
[13] 张勋, 刘韬, 吴连鹏, 等.高效液相色谱-串联质谱法测定多种食品中7种酚类抗氧化剂和对羟基苯甲酸酯类防腐剂[J].食品与发酵工业, 2016, 42(11):206-211.
ZHANG X, LIU T, WU L P, et al.Determination of seven phenolic antioxidants and of p-hydroxybenzoate antiseptics in various foods by LC-MS/MS method[J].Food and Fermentation Industries, 2016,42(11):206-211.
[14] 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):1147-1154.
CHEN X H, ZHAO Y G, YAO S S, et al.Simultaneous determination of nine preservatives and sweeteners in yellow wine and wine by ultrafast liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography, 2011, 29(12):1147-1154.
[15] 李青, 蓝梦哲, 宋光林, 等.液相色谱-串联质谱法测定焙烤食品中多种防腐剂含量[J].食品与发酵工业, 2020, 46(11):283-287.
LI Q, LAN M Z, SONG G L, et al.Detection of preservative contents in baked foods by liquid chromatography-tandem mass spectrometry[J].Food and Fermentation Industries, 2020, 46(11):283-287.