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) Abstract: The purpose of the establishment of God Vitex capsule Jujuboside A method for the determination. Methods HPLC, column: kmmasilC18 column; mobile phase: acetonitrile water (33:67), evaporative light scattering detector; flow rate: 1.0mL · min ~; air: 2.5mL · rain ~; drift tube temperature 110 ℃. Results Jujuboside A reference substance in the sample volume range of 0.24 ~ 6.0g was a good linear relationship (r a 0.999O), the average recovery rate was 98.0, RSD is 3.1 (a 7). Conclusion The method is easy and accurate determination of God Vitex capsule Jujuboside A levels. Keywords: God Vitex capsule; Jujuboside A; determination doi: 10.3969 / j. issn. Key words in the circle 1004-2407.2010.01.017: R927.2 Document code: A Article ID :1004-2407 (2010) 01-0030-02 Vitex capsule collection of God contained in the State Food and Drug Administration standards WS_5449 ( B-0449) for a 2002, by the Suanzaoren, oysters, Anemarrhena, Ophiopogon japonicus, the system Polygonum, Schisandra, Salvia, Poria made, with the raising of Anshen efficacy for the treatment of heart yin deficiency due to poor nerves. Semen is a sedative and hypnotic drugs _1_3 key], in order to ensure the quality of medicines, the author of the determination of Semen preparation methods were studied, with the HPLC method with evaporative light scattering detector in the determination of Suanzaoren Jujuboside A, method is simple and accurate. An instrument and reagent 1.1 Instrument Waters-Alliance2695-2487-type HPLC instrument, AlhechELSD2000 evaporative light scattering detector. 1.2 A reference substance Jujuboside reagent (China Pharmaceutical and Biological Products, batch number 110734-200610); acetonitrile for chromatography pure; water for ultra-pure water; other reagents were of analytical grade; samples (West Anmei Chen medicine Co., Ltd., batch number 080109,080403,[link widoczny dla zalogowanych],080302-2,080302-1,081211,081110). 2 Methods and Results 2.1 column chromatographic conditions kromasilCl. Column (Tianjin Rambo, 250mmX4.6mn2, 5m); column 3O ℃; mobile phase: acetonitrile water (33:67); flow rate: 1.0mL · min ~; air: 2.5 Ⅱ 1L · min; drift tube temperature l10 ℃. 2.2 Preparation of reference substance solution Weigh Jujuboside A precise amount of reference substance, add methanol solution and produced with 0.24mg per 1mL of solution,[link widoczny dla zalogowanych], that is, too. 2.3 Preparation of the test solution of appropriate amount of the contents of this product,[link widoczny dla zalogowanych], small study, accurately weighed 5g; placed in Soxhlet extractor,[link widoczny dla zalogowanych], add about 80mL refluxing ether to nearly colorless (about 3h), discard the ether solution ; dregs remaining ether evaporated to dryness, combined with approximately 80mL of methanol reflux extraction to nearly colorless (about 5h), methanol extract evaporated on a water bath; residue water 20mL, fractional dissolved and transferred to a separatory funnel, water saturated n-butanol extract, 5 times a 15mL, combined butanol extract; butanol saturated with ammonia (30mL concentrated ammonia solution taken diluted with water to 100mL,[link widoczny dla zalogowanych], and then n-butanol saturated, get a lower solution ) washing 2 times, each time 5OmL, washing liquid and discard; butanol butanol saturated with liquid water and then washed 2 times, each time 5OmL, washing liquid was discarded, butanol extract evaporated on a water bath; the residue dissolved in methanol, go to 5mL volumetric flask, diluted with methanol to the mark, shake, as the test solution. 2.4 Preparation of the negative control solution without taking the negative Semen samples of the test solution according to preparation methods, with the rule of law into the negative control solution. Linear range of 2.5 to take Jujuboside A study reference solution (1mL each containing 0.24rag), according to the above chromatographic conditions, respectively, sample 1,2,5,10,15,20 and 25L, chromatographic peak area recorded to peak area and injection volume regression, obtained a regression equation is Y 1.5123X +4.244, r A 0.9990, indicating that Jujuboside A sample volume of between 0.24 ~ 6.0g good linearity. 2.6 The precision of experimental sample solution (batch number 080109), repeated injection 6 times, recording the peak area, the results of RSD was 3.8, indicating good precision of the sample solution. Reproducibility of experimental batches of 2.7 to 080 109 samples taken, determined by the method developed by the body 6, the results of RSD is 3.3.
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