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關(guān)于埃索的液相條件 已有3人參與
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我是參照進口標準:用十八烷基硅烷鍵合硅膠(MicrospherC18.3um,4.6×100nm)為填充劑;以乙腈-磷酸鹽緩沖液(pH7.6,每1L中含磷酸二氫鈉0.0052mol和磷酸氫二鈉0.032mol的溶液)-水(10:10:80)為流動相A;以乙腈-磷酸鹽緩沖液(pH7.6)-水(80:1:19)為流動相B。進行梯度洗脫,流速為1.0ml/min。檢測波長為302nm。用的島津10A的梯度,以這樣的方法做了20天,還是沒做出來,水,乙腈都換了個遍了,鹽也換成了無水的鹽,主峰處仍有干擾,大家是怎么做的呀,可以告訴我嗎? |
金蟲 (正式寫手)
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USP和你的方法流動相比例有點不同。 Phosphate buffer pH 7.6— Dissolve 0.725 g of monobasic sodium phosphate and 4.472 g of anhydrous dibasic sodium phosphate in 300 mL of water, dilute with water to 1000 mL, and mix. Dilute 250 mL of this solution with water to 1000 mL. If necessary, adjust with phosphoric acid to a pH of 7.6. Mobile phase— Prepare a filtered and degassed mixture of Phosphate buffer pH 7.6 and acetonitrile (72.5:27.5). Make adjustments if necessary (see System Suitability under Chromatography 621). [NOTE—To improve the resolution, the composition may be changed to 75:25, if necessary.] 你看看藥典怎么做的:http://dl.vmall.com/c0bmuo0ecy [ Last edited by valley_chow on 2012-12-29 at 14:33 ] |
銅蟲 (小有名氣)

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