Sample aliquots of 159 ml were deri

Sample aliquots of 159 ml were derivatised in a plastic tube protected from light by adding 1.9 ml of distilled water and 0.4 ml of 1 N NaOH. This mixture was allowed to stand for 1 min and then 100 ml of an o-phthalaldehyde methanolic solution (1 g of o-phthalaldehyde l in methanol) was added. The tube was shaken vigorously, the reaction was allowed to proceed for 4 min and then stopped by adding 0.2 ml of 3 N HCl. The derivatised sample solution was centrifuged for 15 min at 8000 rpm,filtered through 0.2-mm millipore syringe filters (Schleicher and Schuell, FP 030/AS, Ref. 462960, ‘s Hertogensbosch, The Netherlands) and analysed by reversed phase-HPLC (RP-HPLC). Separation was carried out on a C column (Spherisorb 2.5 18 mm ODS; 25 cm 3 4.6 mm internal diameter; Chrom pack, Middelburg, The Netherlands). A 20-ml aliquot of injected sample mixture was eluted isocratically over 20 min with a mixture of acetonitrile (40%,HPLC-grade, LAB-Scan, C2502, Dublin, Ireland) and 50 mM NaH PO solution in millipore water 2 4 (60%). The flow-rate was 0.70 ml min . Detection 21
was done with a continuous flow fluorescence meter (Spectra System Series, Thermo Separation Products,FL 3000, Riviera Beach, Florida, USA) with excitation at l 5 350 nm and emission at l 5 450 nm. Alldeterminations were carried out in triplicate.

結果 (中文) 1:

样品的 159 毫升整除的数是 derivatised 在避光通过添加 1.9 毫升蒸馏水和 1 N 氢氧化钠 0.4 毫升的塑料管材。这种混合物被允许站 1 分钟，然后添加邻苯二甲醛甲醇溶液 (1 g 的甲醇中邻苯二甲醛 l) 100 毫升。管被大力震撼了，反应是允许继续 4 分钟，然后通过添加 0.2 毫升 3 N HCl 的停下来。Derivatised 样品溶液离心 15 分钟在 8000 rpm，通过 0.2 毫米微孔注射器过滤器过滤 (施莱歇尔和 FP 030-许尔作为，参考文献 462960 的 Hertogensbosch，荷兰) 和反相-高效液相色谱 (RP-HPLC) 进行了分析。在 C 柱上进行分离 (Spherisorb 2.5 18 毫米耗氧物质; 25 厘米 3 4.6 毫米内径;铬包，米德尔堡，荷兰)。注入的样品混合物 20 毫升分装是洗脱的 isocratically 超过 20 分钟，乙腈 (40%，高效液相色谱级实验室-扫描，C2502，都柏林，爱尔兰) 和 50 毫米 NaH 大埔解决方案在微孔水 2 4 (60%) 的混合物。流动率 0.70 毫升分。检测 21进行与连续荧光流量计 (光谱系统系列，热分离产品，佛罗里达州 3000，里维埃拉海滩，佛罗里达州，美国) 与在 l 5350 nm 激发和发射性能在 l 5 450 毫微米。Alldeterminations 进行了一式三份。

結果 (中文) 3:

159毫升的样品衍生化塑料管中加入1.9毫升蒸馏水和0.4毫升1 N NaOH避光。这种混合物被允许站1分钟，然后100毫升的邻苯二甲醛甲醇溶液（1克邻苯二甲醛在甲醇）加入。该管被剧烈地震动，反应被允许进行4分钟，然后停止加入3毫升0.2盐酸。衍生的样品溶液在8000转离心15 min，经0.2毫米微孔注射器过滤器（Schleicher和许尔，FP 030 /，文献462960的hertogensbosch，荷兰）和反相高效液相色谱法（HPLC）分析。分离是在C柱上进行（Spherisorb ODS 2.5 18毫米；4.6毫米的内部直径25厘米3；铬包，米德尔堡，荷兰）。一个注入的样品混合20毫升等分为洗脱洗脱20分钟以上用乙腈（40%，HPLC级，实验室检查，c2502，都柏林，爱尔兰）和50毫米不宝溶液在微孔水2 4（60%）。流速为0.70毫升。检测21采用连续流动荧光计（光谱系统系列、热分离产品，FL 3000，里维埃拉海滩，佛罗里达州，美国）在L 5 L 5排放在350 nm和450 nm激发。alldeterminations份进行了。