Dent R G, Glaze L
J Assoc Off Anal Chem. 1985 Sep-Oct;68(5):899-901.
The present method for filth in underground marjoram is conducted in 2 parts. The first of these, which is for heavy filth and sand, requires the spice to be boiled with petroleum ether, then floated off with chloroform and, if needed, carbon tetrachloride. The second part, which is for light filth, is dependent on completion of the heavy filth section. After the spice is air-dried, the light filth is extracted with heptane and water. The proposed method was developed to make light filth independent of heavy filth analysis, improve filth recoveries, and reduce microscopic examination time. The light filth is extracted by ethanol defatting followed by a combination 15-60% ethanol/mineral oil extraction in a Wildman trap flask. Tween 80-NaEDTA solution is added to the trapping system to reduce the rising of excess plant material to the trap interface. The official method (AOAC 13th edition secs 44.142, 44.120(b)) produced an average of 8 extraction papers per test portion and microscopic examination took an average of 88 min per test portion. The official method gave average recoveries of 14% for rodent hairs and 26% for insect fragments with 2 spike levels of 15 and 30 for each filth element. Recoveries of the 2 levels of each spike were not significantly different (P greater than 0.05). The proposed method gave average recoveries of 73% for rodent hairs and 70% for insect fragments. The proposed method has been adopted official first action to replace AOAC 13th edition secs 44.142 and 44.120(b) for unground marjoram only.
目前检测地下马郁兰中杂质的方法分两部分进行。第一部分针对重度杂质和沙子,要求将香料与石油醚一起煮沸,然后用氯仿漂浮去除,如果需要,再用四氯化碳处理。第二部分针对轻度杂质,取决于重度杂质部分的完成情况。香料风干后,用庚烷和水提取轻度杂质。开发该方法是为了使轻度杂质检测独立于重度杂质分析,提高杂质回收率,并减少显微镜检查时间。轻度杂质通过乙醇脱脂,然后在Wildman捕集烧瓶中用15 - 60%乙醇/矿物油组合提取。向捕集系统中加入吐温80 - NaEDTA溶液,以减少过多植物材料上升到捕集界面。官方方法(《美国官方分析化学师协会第13版》第44.142节、44.120(b)节)每个测试部分平均产生8份提取纸,显微镜检查每个测试部分平均耗时88分钟。官方方法对啮齿动物毛发的平均回收率为14%,对昆虫碎片的平均回收率为26%,每种杂质元素有15和30两个加标水平。每个加标水平的两个回收率无显著差异(P大于0.05)。所提出的方法对啮齿动物毛发的平均回收率为73%,对昆虫碎片的平均回收率为70%。所提出的方法已被官方首次采用,仅用于未研磨的马郁兰,以取代《美国官方分析化学师协会第13版》第44.142节和44.120(b)节。