Sheridan Robert, King Thomas
New York State Department of Agriculture and Markets, Food Laboratory, Building 7, State Office Campus, Albany, NY 12235, USA.
J AOAC Int. 2008 Sep-Oct;91(5):1095-102.
A highly sensitive and selective method that requires minimal sample preparation was developed for the confirmation and quantitation of cyclamate in a variety of foods by high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). Sample preparation consisted of homogenization followed by extraction and dilution of cyclamate with water. HPLC separation was achieved using a bridged ethyl hybrid C18 high-pressure column with a mobile phase consisting of 0.15% acetic acid and methanol. Under electrospray ionization negative conditions, quantitation was achieved by monitoring the fragment m/z = 79.7 while also collecting parent ion m/z = 177.9. Two food matrixes, diet soda and jelly, were subjected to a validation procedure in order to evaluate the applicability of the method. The cyclamate limit of detection for both matrixes was determined to be 0.050 microg/g with a limit of quantitation of 0.150 microg/g. The correlation coefficient of the calibration curves was >0.9998 from 0.0005 to 0.100 microg/mL. The method has been used for the determination of cyclamate in several foods and the results are presented.
开发了一种高灵敏度和高选择性的方法,该方法所需的样品前处理极少,用于通过高效液相色谱/串联质谱法(HPLC/MS/MS)对多种食品中的甜蜜素进行确证和定量分析。样品前处理包括匀浆,然后用水提取并稀释甜蜜素。使用桥接乙基杂化C18高压柱进行HPLC分离,流动相由0.15%乙酸和甲醇组成。在电喷雾电离负离子条件下,通过监测质荷比m/z = 79.7的碎片同时收集质荷比m/z = 177.9的母离子来实现定量分析。对两种食品基质,即无糖汽水和果冻,进行了验证程序,以评估该方法的适用性。两种基质中甜蜜素的检测限均确定为0.050微克/克,定量限为0.150微克/克。校准曲线在0.0005至0.100微克/毫升范围内的相关系数>0.9998。该方法已用于多种食品中甜蜜素的测定,并给出了结果。