Using chiral liquid chromatography-mass spectrometry (LC/MS), a simple and rapid identification test was developed for aminotadalafil [(6R,12aR)-2-amino-6-(1,3-benzodioxol-5-yl)-2,3,6,7,12,12a-hexahydropyrazino[1 ,2 : 1,6]pyrido [3,4-b]indole-1,4-dione; RR-ATDF] and its stereoisomers contained in health foods, e.g. herbal products. A sample solution was prepared using methanol extraction. Analysis was performed on a chiral column with the mixture of 0.1% formic acid/acetonitrile (7 : 3) as mobile phase at 30• C. Each resolution value of four stereoisomers of ATDF was greater than 1.3. A mass spectrometer was used as a detector to enhance specificity by excluding the effects of general components derived from the sample. The four individual stereoisomers of ATDF in the health foods were identified based on their respective retention times. Results showed that structural conversions of RR-ATDF into (6R,12aS)-2-amino-6-(1,3-benzodioxol-5-yl)-2,3,6,7,12,12a-hexahydropyrazino[1 ,2 : 1,6]pyrido [3,4-b]indole-1,4-dione (RS-ATDF) and (6S ,12aS)-2-amino-6-(1,3-benzodioxol-5-yl)-2,3,6,7,12,12a-hexahydropyrazino[1 ,2 : 1,6]pyrido [3,4-b]indole-1,4-dione (SS-ATDF) into (6S ,12aR)-2-amino-6-(1,3-benzodioxol-5-yl)-2, 3,6,7,12,12a-hexahydropyrazino[1 ,2 : 1,6]pyrido [3,4-b]indole-1,4-dione (SR-ATDF) occurred under strongly basic conditions, which indicates that such conditions must be avoided during sample preparation. Using this method, RR-ATDF and SR-ATDF were detected in a health food; this is the first report describing that ATDF diastereomers are present in health foods.
A simple and rapid method for screening of drugs in health foods using 2-dimensional TLC was established. The development systems were: (1) ethyl acetate/methanol/28% ammonia (85:10:5), (2) cyclohexane/toluene/diethyl amine (65:25:10), (3) methanol and (4) ethyl acetate/methanol/25% ammonia (85:10:5). System (1) and (2) were run as 2-dimensional high-performance TLC, and System (3) and (4) were run as 2-dimensional conventional TLC. Sample extracted with methanol from health foods was applied to standardized two 2-dimensinal TLCs and 4 Rf values obtained from 4 development systems were compared with reference Rf values which were measured previously using standard materials. The repeatability of reference Rf values were secured by standardizing development conditions and pattern of 4 Rf values was speciˆc for 80 drugs. Moreover, using 2-dimensinal TLC enable to assign 4 Rf values to unknown substance without in‰uence of matrix from health foods, so it was possible to determine drugs comparing 4 Rf values. This method could be applied asˆrst screening test for prevention of health crisis occurred by drugs added to health foods illegally.
When fluid is mixed by a rotor and small vessel that has a narrow clearance between its wall and the rotor with the upper part covered by an endplate, the processing fluid becomes a high-speed thin-film spin flow. This flow possibly allows the peripheral speed to be over 30 m/s, which was unable to be obtained by a conventional high-speed mixer. As a result, the processing fluid obtains more and homogenous energy. In an actual experiment, we compared a high-speed thin-film spin mixer with a conventional high-speed mixer upon an emulsification experiment with soybean oil. The experiment proved that the former mixer could control the particle size distribution. It also proved that the same result could be obtained by continuous operation as by batch operation. In conclusion, the high-speed thin-film spin mixer can control particle size distribution with a high efficiency.A rapid and simple method using gas chromatography (GC) for the determination of diethylene glycol (DEG) in toothpaste was developed. DEG in toothpaste was extracted with methanol containing 1,4-butanediol as the internal standard by using an ultrasonic bath. The centrifuged and filtrated methanol extracts were analyzed by GC on an InertCap 624 capillary column. The recoveries of DEG from toothpaste fortified at the levels of 0.1, 0.5 and 1.0%, were 103.6, 99.9, 99.4%, respectively. The quantitation limit of DEG in toothpaste was 0.05??%. The proposed method could be applied to other cosmetics on the market without any interference. By using this method, DEG was detected the presence in two out of 10 toothpaste samples set to the hotel. This analytical method should be useful for quality control for manufacturers and importers of cosmetics.
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