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The HPLC system consisted of two Rainin HPX pumps (10 ml head), aRheodyne injector (model 7125) with a 20-ul loop, an LDC FluoromonitorIII, and a Hewlett-Packard recorder-integrator (model 3390A). The column used for the quantitation of EQ was a reversed-phase C18 (5 um 4 mm ID x 15 cm) (SGE, Austin, Tex.) protected with a guard column filled with Perisorb RP 18 (Upchurch Scientific). The mobile phase was acetonitrile-10 mM ammonium phosphate, monobasic, containing 1 mM tetrabutyl-ammonium hydrogen sulfate and adjusted to pH 5.9 with solid ammonium hydrogen carbonate (7:3, v/v) and the flow rate was 0.9 ml/min.The ammonium phosphate buffer was prepared every 5 d. The analyses were performed at ambient temperature; the detector range was set at 20-100 and the injection volume ranged 0.5-20ul according to the concentration of EQ in the sample. EQ HCI was prepared as described (Kim, 1985) by converting the available dark oily EQ (a gift from Monsanto) into crystalline EQ HCI and was recrystallized several times from methanol-acetonitrile to give a colorless analytical sample (mp 192-193°C). The standard solution was prepared weekly in methanol (10 mg/ml) and immediately diluted with acetonitrile to 0.1 ug/ml and kept in the dark at room temperature. [ Last edited by zl0921516 on 2012-5-31 at 14:55 ] |
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榮譽版主 (文壇精英)
| HPLC系統(tǒng)包括兩個的RAININ黃嘌呤泵(頭10毫升),20-UL循環(huán)aRheodyne噴油器(型號7125),最不發(fā)達國家FluoromonitorIII和惠普錄像機集成(型號3390A)。情商的定量分析中使用的列是1反相C18(5微米編號4毫米x 15厘米)(上海黃金交易所,奧斯汀,得克薩斯州),填補了保護柱與RP的18 Perisorb(厄普丘奇科技)保護。流動相為乙腈-10毫米的磷銨,一元,含1毫米的四丁基硫酸氫銨固體碳酸氫銨(7:3,V / V),流速和調(diào)整pH值5.9,0.9毫升/分鐘。磷銨緩沖區(qū)準備每5天。在室溫下進行的分析檢測范圍在20-100和注射量介于0.5-20ul根據(jù)樣品濃度的EQ設(shè)置。 情商人機交互所述結(jié)晶情商人機交互轉(zhuǎn)換成可用暗油性的EQ(從孟山都公司的禮物)(金,1985年)和甲醇 - 乙腈重結(jié)晶數(shù)次給無色的分析樣品制備(熔點192-193°C間)。標準的解決方案,準備每周甲醇(10毫克/毫升),并立即用乙腈稀釋0.1微克/毫升,室溫保持在黑暗中。 |

榮譽版主 (文壇精英)
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高效液相色譜系統(tǒng)由兩個 Rainin HPX(泵品牌)泵(10ml泵頭),一個Rheodyne進樣器(7125型)連帶一根20-ul進樣針,一個LDC熒光檢測器III,以及惠普牌記錄積分器( 3390A型)。用于測定EQ的柱子是C18(5 um 4 mm ID x 15 cm) (SGE, Austin, Tex.) 反相柱子,用Perisorb RP 18 (Upchurch Scientific)填充的保護柱保護 。流動相是乙腈-10 mM 磷酸銨溶液,一元堿,包含1 mM四丁基硫酸氫銨溶液并用碳酸氫銨(7:3, v/v)調(diào)ph至5.9,流速 0.9 ml/min。磷酸銨緩沖液每隔5天配制一次。室溫下進行檢測分析,檢測波長范圍設(shè)置為20-100nm,根據(jù)樣品中EQ的濃度進樣量的范圍為 0.5-20ul。 EQ HCI 根據(jù) (Kim, 1985)所述進行制備:通過將可用黑油EQ(孟山都產(chǎn)品)轉(zhuǎn)換成EQ HCI 晶體,并用甲醇-乙腈重結(jié)晶幾次得出無色的分析樣品 (mp 192-193°C). 標準品溶液用甲醇配制,并立即用乙腈稀釋至 0.1 ug/ml,室溫下暗中保存,每周配制一次。 mM是mg/mls的意思 |

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