Tsuruda Sayuri, Sakamoto Tomonori, Akaki Kouichi
Fukuoka City Institute for Hygiene and the Environment, 2-1-34 Jigyohama, Chuo-ku, Fukuoka 810-0065, Japan.
Shokuhin Eiseigaku Zasshi. 2013;54(3):204-12. doi: 10.3358/shokueishi.54.204.
A rapid and simple method for the simultaneous determination of twelve sweeteners and nine preservatives in various foods by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. The sweeteners and preservatives were extracted from solid samples with 80% and 50% methanol and from liquid samples with 80% methanol, followed by Oasis WAX cartridge cleanup. The LC separation was performed on a XSelect CSH Phenyl-Hexyl column (5 μm, 2.1 mm ×150 mm) with a mobile phase of 10 mmol/L acetate buffer (pH 4.0)-acetonitrile and MS detection with negative ion electrospray ionization. The quantification limits of acesulfame K (AK), alitame (AL), aspartame (ASP), cyclamic acid (CYC), neotame (NEO), saccharin Na (SAC), p-hydroxybenzoic acid methyl (PHBA-Me), p-hydroxybenzoic acid ethyl (PHBA-Et), p-hydroxybenzoic acid isopropyl (PHBA-iPr), p-hydroxybenzoic acid propyl (PHBA-Pr), p-hydroxybenzoic acid isobutyl (PHBA-iBu) and p-hydroxybenzoic acid butyl (PHBA-Bu) were 0.001 g/kg, those of dulcin (DU), glycyrrhizic acid (GLY), neohesperidin dihydrochalcone (NHDC), rebaudioside A (REB), stevioside (STV), sucralose (SUC) and benzoic acid (BA) were 0.005 g/kg, and those of sorbic acid (SOA) and dehydroacetic acid (DHA) were 0.02 g/kg. The mean recoveries from ten kinds of foods fortified at the levels of 0.02 and 0.2 g/kg were 70.9-119.0%, and their relative standard deviations were 0.1-11.7%.
建立了一种快速简便的液相色谱-串联质谱法（LC-MS/MS）同时测定各类食品中12种甜味剂和9种防腐剂的方法。甜味剂和防腐剂从固体样品中用80%和50%的甲醇提取，从液体样品中用80%的甲醇提取，然后用Oasis WAX柱净化。液相色谱分离在XSelect CSH苯基-己基柱（5μm，2.1mm×150mm）上进行，流动相为10mmol/L乙酸盐缓冲液（pH 4.0）-乙腈，质谱检测采用负离子电喷雾电离。乙酰磺胺酸钾（AK）、阿力甜（AL）、阿斯巴甜（ASP）、环己基氨基磺酸（CYC）、纽甜（NEO）、糖精钠（SAC）、对羟基苯甲酸甲酯（PHBA-Me）、对羟基苯甲酸乙酯（PHBA-Et）、对羟基苯甲酸异丙酯（PHBA-iPr）、对羟基苯甲酸丙酯（PHBA-Pr）、对羟基苯甲酸异丁酯（PHBA-iBu）和对羟基苯甲酸丁酯（PHBA-Bu）的定量限为0.001g/kg， dulcin（DU）、甘草酸（GLY）、新橙皮苷二氢查耳酮（NHDC）、莱鲍迪苷A（REB）、甜菊糖苷（STV）、三氯蔗糖（SUC）和苯甲酸（BA）的定量限为0.005g/kg，山梨酸（SOA）和脱氢乙酸（DHA）的定量限为0.02g/kg。在0.02和0.2g/kg水平下对10种食品进行加标回收试验，平均回收率为70.9-119.0%，相对标准偏差为0.1-11.7%。
