CN86102668A - 含有示踪剂的微量配料 - Google Patents
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Abstract
用以测定成批物质中所含微量配料浓度的示踪粒,现予透露。示踪粒的构成一是细末铁磁散物,其中百分之九十约为筛目325或更细小,一是微量配料,一是粘合剂。微量配料和铁磁物都粘合于粘合剂中;示踪粒的大小约为筛号35至80之间。
Description
本发明涉及申请人原已享有的美国专利第2,868,644、3,469,990、4,152,271和4,188,408号。许多微量配料,如药物、菅养素或其他次要的官能性配料,为了保证质量或遵守规章的要求,往往需要加以分折。本发明提供一项方法,它能在含有几种配料的均匀混合物中,方便而有效地测出这整批物质中所含具体微量配料的数量。
在一整批物质中,通常需要检验某一微量配料的相对数量,如药物或营养素,其原因有几种。美国粮食和药物管理局规定,在一些动物饲料中只可添加亚硒酸钠或硒盐的硒预拌剂,预拌剂的硒含量不得超过200PPM。饲料中含低浓度的硒(5PPM)即有剧毒,粮食和药物管理局要求每批动物饲料预拌剂的硒含量,必须加以定量分析。这一任务显然十分繁重和耗费时间。如果开拓一种方法,使某具体的微量配料能随时随地分离出整批物质之外,然后在下受该批物质的干扰下进行分析,其用途显然很大。对硒来说,用这种方法可以测定硒的含量是否符合粮食和药物管理局所允许的亚硒酸或硒酸盐的含量标准。已有分析程序尚不能从其他硒化合物中辨别出亚硒酸和硒酸盐,而这些硒化合物可能已在或已加到动物饲料预拌剂中。这种方法也能辨别不同来源的同类药物或营养素。
为了实现上述方法,申请人首次在美国专利第4,152,271号中披露了一种铁磁示踪料,它可以利用磁分离器把铁磁示踪料从成批的预拌剂中分离中来,而比起过去用的示踪剂要迅速和简易得多。使用这些物质具有的各种优点十分明显。用一个磁性分离器配合使用这种示踪粒,可以检测成批物质中的大件抽样,而用沉积分离法只能限于检测小件抽样。
申请人在原来的美国专利第4,152,271号公开的示踪剂载体含有软铁末或其他可在磁场中磁化的,但离开磁场即失去磁性的铁磁物。铁磁物可吸附上食品,药品和化妆品用色,或其他经许可而便于识别的微量配料,以便铁磁粒易于被辨认。由于示踪粒是要经过点数的,所以这成批物质即便受到磨蚀或渗滤,使用于识别的吸附层受到重大损伤,仍不致影响到示踪粒点数的准确性。
本发明的目的是要把微量配料渗合示踪粒中,当示踪粒从成批物质中分离出来时,基本上百分之百的具体微量配料也同时分离了出来,也就是从成批物质中释放了出来。
此项发明的另一目的是提出一种示踪微粒,它可在成批物质中染载上微量配料,它又能加以回收,用作分析试验面微量配料基本上不致无缘无故地从示踪粒中分离出去。
一种测定成批物质中所含微量配料浓度的示踪粒。示踪粒的构成,一是精细的铁磁散式物质,其中约百分之九十达到筛目325左右或更细一些,一是微量配料,一是粘合剂,用以粘合微量配料和铁磁物。示踪粒的大小约为筛号35至80。
如前所说,所谓微量配料可以是一种药物,一种主要营养素或其他临界物质,而必需进行分析以保证质量,或以应规章所需求。用磁吸从一成批物质中回收含有微量配料的示踪剂,可取得相对纯净的剂体,而不致受成批物质通常产生的分析性干扰。这一具体示踪剂一经分离出来后,极易辨认,其办法可用化学分析法,也可在示踪粒上加色号,用物理方法加以辨认。磁铁物质可以用还原铁,电解铁或其他一些在磁场磁化,但离开磁场磁性即告消失的磁铁物质。但这样磁物质的大小必须十分小于示踪粒。这样,每一粒示踪粒才能含有足够数量的磁物质,以利于用磁吸来回收示踪剂。示踪剂中可含有百分之十的磁铁物质。但为了使用申请人原先的专利发明所透露的一些分离技术,示踪粒应包含有大约百分之二十五至三十五的磁铁物质才能成为优选的方法,示踪粒从成批拌剂中的回收率可超过百分之九十。如运用美国专利序列号4,152,271中透露的陶瓷瓶技术,下列数据即为示踪剂按其铁的功能,可回收的百分比:
铁百分比 回收百分比
4% 1.0%
8% 7.9%
16% 18.5%
25% 90.9%
32% 95.1%磁铁物质最好较为细小,至少有百分之九十的磁铁末能通过美国标准筛325目。使用这样细的末粒,其合成的示踪剂的每一散式单位便可合理地分布有合乎比例的磁铁物质。
为有助于视力测定,较为优选的方法是在合成示踪剂中使用色号添加剂。可使用各种惰性色号添加剂,如着色矾土或淀粉末。较好的添加剂的组成是细末硅胶,约筛目170到325,染以食品、药物和化妆品色。
此项发明的主旨是提出一种示踪剂,这种示剂物把不同的组成部分如磁铁物质和微量配料粘合在一粘合基体中。典型地,用于压制药片或其他丸片的粉末所用的凝胶或熟淀粉,可作为合适的粘合剂。如不用于食物或动物饲料,也可用合成塑料、丙烯或环氧物来做粘合物质。
最适宜于做粘合和基体的物质是含有百分之十蛋白质的上等的纯净面粉。标准的和面设备可用来搅拌含有的配料的面团,捍压面团成薄片或空心面,并把捍压成的面团进行干燥处理。下一步便是用锤磨机以粉碎,研成末,再过筛成为示踪主体。最好筛选示踪粒成筛35至80目左右大小。碎屑和粗粒还可重复使用。在上述大小范围内,示踪产物将为每克含有五万至七万左右的个别微粒。
例1
下列配料可用家用电搅拌器搅拌
面粉(通用) 321.1克
还原铁(325目筛) 125克
硅胶(红色) 10克亚硒酸钠43.9克溶于160毫升水的溶液。将溶液加在上述配料中不断搅拌,最后成为极其干的面团。按来样湿度计算,这拌和体为500克的‘干燥’物质,其中25%是还原铁,2%是带色号硅胶和8.78%的亚硒酸钠(4%的硒)。
面团随后用装有3/32″面平板的磨肉机挤压,再把经过挤压的面团加以干燥到约湿度10%,再通过装有1/16″筛网的锤磨机。锤磨后进行筛选。筛号35到80之间的产品占30%。每一毫克成品含有粒子62.8粒。
例2
用例1中办法取得的示踪剂10毫克,搅拌于禽食浆100克中调制成预拌硒,其中每百万份示踪剂中含硒一百份,相当于亚硒酸钠四份。打开磁性分离器,示踪剂通过一次后,即可回收9.1毫克。回收的示踪剂分布在15毫升的水中,再加以过滤。把10毫升的试样倾入一个瓶子里,瓶内装有大约20毫升0.0075N的硫代硫酸钠正常溶液,把两者加以混合。加三滴1%的淀粉浆作为指示剂,然后再加上1毫升5%浓度的盐酸。该溶液立即用0.005N的碘正常溶液进行滴定。
由于亚硒酸钠同硫代硫酸盐结合为稳固的络合物,过剩的硫代硫酸盐又再次用碘滴定,这一预拌体可含有3.6±0.02PPM的硒。
这种简易迅速的滴定验定法一般虽然不能用于络合物的基体如动物饲料或预拌剂上。但这种验定法却可用于此处,因为分析试样已从饲料预拌剂中相当纯净地分离了出来。硒虽然是一种必需的营养素,但具剧毒,其毒性低达其营养的十三至四十倍,因此粮食和药物管理局要求对每一批硒预拌剂进行测定,以减少发生灾难性差错的可能性。采用此项发明便有可能对这些微量配料进行简易、迅速、具体而化费不大的测定。
发明当然还可进而用于其他通常不易测定的微量配料,如nicarba_zin和维生素K和D,也可用于鉴别不同产家的同类专利产品。
Claims (15)
1、用以测定成批物质中所含微量配料浓度的示踪粒,其特征在于,该示踪粒包括一种细微的铁磁散物质,其中90%左右为筛目325或小于325目,一种微量配料和一种粘合剂,该微量配料和铁磁物质被粘在该粘合剂中,上述示踪粒的大小约为筛目35至80。
2、按权利要求1所述的示踪粒,其中所述的铁磁散物质,其含量按重量算为25%至35%左右。
3、按权利要求1所述的示踪粒,其中还含色号添加剂。
4、按权利要求1所述的示踪粒,其中所述的微量配料硒为亚硒酸钠或硒酸盐。
5、按权利要求1所述的示踪粒,其中所述的粘合体含有下列各种物质中的一种:面粉、凝胶、淀粉、塑料、丙烯或环氧物。
6、按权利要求3所述的示踪粒,其中所述的色号添加剂含有带色硅胶。
7、按权利要求3所述的示踪粒,其中所述的色号添加剂含有细末粒,1其大小约在筛目170至325之间。
8、一种基本均匀的组合物,该组合物大部份是散装配料,小部分是示踪粒,其特征在于,该示踪粒包含有细末的铁磁物,其中约90%的是325筛目或小于325目,还有微量配料和一粘合剂,粘合剂把上述微量配料和铁磁物质粘合在一起,示踪粒的大小约为筛目35至80之间。
9、按权利要求8所述的组合物,其中所述的铁磁散物在上述示踪粒中,按重量计约为25%至35%。
10、按权利要求8述的组合物,其中所述的示踪粒还含有色号添加剂。
11、按权利要求10所述的组合物,其中所用的添加剂系药物。
12、按权利要求8所述的组合物,其中所用的微量配料含有亚硒酸钠或硒酸钠中的硒成份。
13、按权利要求8所述的组合物,其中所用的粘合剂含有下列几种物质中的一种:面粉、凝胶、淀粉、塑料、丙烯或环氧。
14、按权利要求10所述的组合物,其中所用的色号添加剂包括带色硅胶。
15、按权利要求10所述的组合物,其中所用的色号添加剂的构成是细末粒子,其大小约为筛目170至325之间。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US06/723,753 US4654165A (en) | 1985-04-16 | 1985-04-16 | Microingredient containing tracer |
US723.753 | 1985-04-16 |
Publications (2)
Publication Number | Publication Date |
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CN86102668A true CN86102668A (zh) | 1986-10-15 |
CN1003448B CN1003448B (zh) | 1989-03-01 |
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Application Number | Title | Priority Date | Filing Date |
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CN86102668.3A Expired CN1003448B (zh) | 1985-04-16 | 1986-04-15 | 含有示踪剂的微量配料 |
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Country | Link |
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US (1) | US4654165A (zh) |
EP (1) | EP0198426B1 (zh) |
CN (1) | CN1003448B (zh) |
DE (1) | DE3664686D1 (zh) |
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- 1986-04-10 DE DE8686104912T patent/DE3664686D1/de not_active Expired
- 1986-04-15 CN CN86102668.3A patent/CN1003448B/zh not_active Expired
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CN104903724A (zh) * | 2012-11-15 | 2015-09-09 | 麦克罗-奇瑟斯公司 | 示踪物粒子及其制备方法 |
US10175199B2 (en) | 2012-11-15 | 2019-01-08 | Micro-Tracers, Inc. | Tracer particles, and methods for making same |
Also Published As
Publication number | Publication date |
---|---|
EP0198426B1 (en) | 1989-07-26 |
CN1003448B (zh) | 1989-03-01 |
DE3664686D1 (en) | 1989-08-31 |
EP0198426A1 (en) | 1986-10-22 |
US4654165A (en) | 1987-03-31 |
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