荧光光度法直接测定环境水中的苯酚和苯胺

了用荧光分光光度法通过控制酸度直接测定环境水中苯酚和苯胺两种水中污染物的新方法。在ｐＨ＝１时，直接测定苯酚的含量，波长为λｅｘ／λｅｍ＝２７０／２９７ｎｍ，检出限为４．０ｎｇ／ｍＬ，线性范围为０～３．２μｇ／ｍＬ。在ｐＨ＝１２时，直接测定苯胺的含量，波长为λｅｘ／λｅｍ＝２８０／３４０ｎｍ检出限为４．３ｎｇ／ｍＬ，线性范围为０～２．０ｕｇ／ｍＬ，回收率达９９～１０１％。     

超高压液相色谱荧光检测法快速测定水中痕量苯胺与联苯胺

建立了直接进样/超高压液相色谱荧光检测法快速分析水中苯胺和联苯胺的新方法。通过研究流动相、水样pH值、水样电导率和滤器材质的影响,确定了最优化的实验方案。水样直接通过0.22μm微孔滤膜(聚四氟乙烯材质)过滤,以乙腈-3.85 g/L醋酸铵(25∶75)为流动相,荧光检测器(苯胺λex/λem=232nm/329 nm,联苯胺λex/λem=292 nm/383 nm)在0.8 min内完成分析。苯胺和联苯胺在1.0～100.0μg/L范围内线性关系良好,相关系数均大于0.999,仪器精密度(n=10)分别为0.4%和0.5%,方法检出限(S/N=3)分别为0.023μg/L和0.024μg/L,方法定量下限(S/N=10)为0.078μg/L和0.079μg/L,方法回收率为86%～106%。该方法具有前处理简单、方法检出限低、分析速度快等优点,适用于水体中苯胺和联苯胺的快速检测。     

高效液相色谱荧光检测法分析氨基酸

氨基酸的分析方法应用最普遍的是离子交换色谱法。在-SH存在下,邻苯二甲醛(OPA)与伯氨基在柱后反应产生荧光物质进行氨基酸的检测是一种有效的微量分析法。而亚氨酸则须先用次氯酸钠氧化再与OPA反应。整个系统如图1如示。我们应用此法分析了谷物的总氨基酸和茶叶中的游离氨基酸含量。     

高效液相色谱-荧光检测法测定葡萄酒中总亚硫酸盐

 摘要：建立了测定葡萄酒中总亚硫酸盐的高效液相色谱方法。N-（9-吖啶基）马来酰亚胺与样品中亚硫酸盐反应生成一种较强的荧光络合物,利用荧光检测器进行检测。方法具有样品用量少、操作简便、灵敏度高等特点,回收率为98.0％～103.0％,相对标准偏差小于4.6％。     

液相色谱-质谱法测定水中的苯胺

按照HJ68-2010,建立了液相色谱-质谱法测定水中苯胺的方法.在优化条件后,该方法展示了优异的性能:(a)在10～ 200μg/L范围内具有良好的线性关系,相关系数R为0.9997; (b)与其它方法相比,有较低的检出限,检出限仅为2.0μg/L;(c)精密度和准确度较好,相对标准偏差RSD<6%,空白水样加标回收...     

高效液相色谱荧光检测法测定药物中的氯乙酰氯

建立测定药物中氯乙酰氯含量的高效液相色谱–荧光检测方法。以吖啶酮乙酰肼为荧光标记试剂,对氯乙酰氯进行柱前衍生。在室温下反应15 min,衍生产率达到最大。衍生溶液在XDB–C18柱上,以水和乙腈为流动相进行分析,激发波长和发射波长分别为255 nm和429 nm。氯乙酰氯浓度在1~1 000 nmol/L范围内与色谱峰面积具有良好的线性关系,线性相关系数r=0.999 9。方法的检出限为0.35 nmol/L,仪器精密度和方法精密度分别为0.52%和0.67%(n=6)。样品加标回收率为92.5%~95.6%。该方法简单、准确,精密度良好,可用于测定药物中氯乙酰氯的残留量。     

高效液相色谱—荧光检测法测定蒽和荧蒽

采用高效液相色谱－荧光检测法测定多环芳烃化合物蒽和荧蒽。在Ｓｈｉｍ－ｐａｃｋ ＣＬＣ－ｐｌｅｎｙｌ柱上，以５０％的乙腈水溶液作流动相，１２ｍｉｎ内实现了两组分的同时分离测定。线性范围为０－８０μｇ／ｍＬ，检测限低于５０ｎｇ／ｍＬ，相对标准偏差小于１％。     

高效液相色谱-荧光检测法测定水果中乙氧基喹啉

建立了高效液相色谱-荧光检测联用测定苹果、梨、葡萄、橙子等水果中乙氧基喹啉的方法。样品经与维生素C混合制样后,加0.1 mol/L氢氧化钠调至pH 11～12后,以正己烷提取2次。提取液浓缩后用乙腈复溶,采用高效液相色谱荧光检测器测定,外标法定量。结果表明,乙氧基喹啉在2～100μg/L范围内呈良好的线性关系,相关系数(r)为0.999 99;方法检出限和定量下限分别为0.01、0.02 mg/kg;在0.02、0.04、0.2、1 mg/kg加标水平下的平均回收率为80.4%～108%,相对标准偏差(RSD,n=6)为1.4%～8.1%。该方法简单快速、重复性好、稳定性强,适用于水果样品中乙氧基喹啉的定性定量检测。     

高效液相色谱-荧光检测法测定食品接触材料塑料制品中荧光增白剂

建立了同时测定食品接触材料塑料制品(食品包装袋)中荧光增白剂的高效液相色谱-荧光检测法。样品用20 mL三氯甲烷作提取剂,超声提取30 min,提取温度为40 ℃,用高效液相色谱进行定性定量分析。采用Eclipse XDB-C18(250 mm×4.6 mm, 5 μm)为分析柱,以5 mmol/L乙酸铵溶液和乙腈为流动相,梯度洗脱,荧光激发波长为350 nm,发射波长为430 nm。结果显示,4种荧光增白剂4,4′-双［2-(邻氰苯基)乙烯基］苯(1,4-bis(4-cyanostyryl)benzene, C.I. 199)、1,4-双(2-苯并恶唑)萘(1,4-bis (2-benzoxazolyl)naphthalene, C.I. 367)、4,4′-双(2-甲氧苯乙烯基)联苯(4,4′-bis(2-methoxystyryl)biphenyl, C.I. 378)和2,5-双(5-叔丁基-2-苯并恶唑基)噻吩(2,5-thiophenediylbis (5-tert-butyl-1,3-benzoxazole), C.I. 184)可以较好地分离;检出限(S/N=3)分别为0.3、0.1、0.05、0.14 mg/L,定量限(S/N=10)分别为1.0、0.4、0.2、0.5 mg/L,回收率范围为78.9%～101.1%,相对标准偏差小于10%,线性关系良好。该法简便、结果准确、灵敏度高,能够满足进出口食品包装材料塑料制品中荧光增白剂的日常检测。     

高效液相色谱/安培检测法测定蜂蜜中苯酚残留量

研究了用高效液相色谱 /安培检测法测定蜂蜜中苯酚残留量。考察了试验参数对测定结果的影响。在所选试验条件下 ,苯酚保留时间约为 12min ,检出限为 2 .0ng·g- 1。三组不同水平的加样回收率为 91.6 10 1.9% ,相对标准偏差 2 .812 .8%。测定结果满意     

水环境中酚、二元酚和三元酚的高效液相色谱分析

采用固相萃取法富集水样，研究了水环境中苯酚、二元酚和三元酚类化合物的反相高效液相色谱分析法。     

Determination of paralytic shellfish poisoning toxins in cultured microalgae by high-performance liquid chromatography with fluorescence detection

A novel method for the determination of paralytic shellfish poisoning (PSP) toxins using high-performance liquid chromatography with fluorescence detection was developed. The fluorescent derivates of neosaxitoxin (neoSTX), saxitoxin (STX), gonyautoxins 1 and 4 (GTX1+4), and gonyautoxins 2 and 3 (GTX2+3) were separated on a μBondapak NH₂ column (300 mm × 3.9 mm, 10 μm) using water and acetate buffer (pH 6.5) as the mobile phase (1.00 mL min⁻¹) in gradient mode with fluorescence detection at 390 nm (excitation at 330 nm). The linear ranges of neoSTX, STX, GTX1+4 and GTX2+3 were 3.31–331, 0.952–95.2, 3.78–378 and 0.124–12.4 ng mL⁻¹, respectively. The detection limits of neoSTX, STX, GTX1+4 and GTX2+3 were 1.10, 0.32, 1.26 and 0.041 ng mL⁻¹, respectively. The method was successfully applied to the determination of PSP toxins in microalgae. The recoveries ranged from 88±2% to 107±4% and the relative standard deviations were 0.16% to 4.4%. The procedure is also environmentally friendly because no organic solvent is used in the mobile phase.     

高效液相色谱法与酶联免疫试剂盒测定海水中痕量氯霉素

详细报道了海水样品中氯霉素的高效液相色谱检测方法及酶联免疫试剂盒检测方法。应用高效液相色谱法测定海水中氯霉素,方法的线性范围为5～50ng,检出限为0．064ng,回收率为96．2％-118．4％,相对标准偏差小于8．9％。酶联免疫试剂盒测定海水中的氯霉素背景值偏高,在加标浓度为10ng／mL时回收率为101．0％,相对标准偏差为8．32％。     

Rapid determination of nitrite in foods in acidic conditions by high‐performance liquid chromatography with fluorescence detection

In this study, a simple, rapid, and sensitive method for the determination of nitrite (NO₂^?) in food samples by high‐performance liquid chromatography with fluorescence detection in acidic conditions had been developed. The derivatization of the nitrite with 2,3‐diaminonaphthalene was performed in acidic conditions to yield the highly fluorescent 2,3‐naphthotriazole, which was directly analyzed by high‐performance liquid chromatography with fluorescence detection without adjusting the solution to alkaline. The analysis column was reversed‐phase C₈ column. A constant flow rate of 1.0 mL/min was employed using water/acetonitrile as the mobile phase in isocratic mode (70:30, v/v). Fluorescence was monitored with excitation at 375 nm and emission at 415 nm. The standard calibration curves were linear for nitrite in different matrixes in the concentration range of 0–100 μg/L, and the correlation coefficients ranged from 0.9978 to 0.9998. The limits of detection and quantification were in the ranges of 0.012–0.060 and 0.040–0.20 mg/kg, respectively. The recoveries of nitrite from samples spiked at three different concentrations were 74.0–113.2%, and the relative standard deviations of the recovery results (n = 6) were 1.67–10.8%. The proposed method has good repeatability and is very sensitive and simple. It has been successfully used to determine nitrite in foods.     

高效液相色谱法测定食品接触材料中苯酚和4-叔丁基苯酚迁移量

提出了食品接触材料在水、3％(质量分数)乙酸溶液、乙醇(1+9)溶液、异辛烷4种食品模拟物中苯酚、4-叔丁基苯酚迁移量的高效液相色谱测定方法.不同种类的食品模拟物采用不同的样品前处理方法提取后,用Diamonsil C18色谱柱为固定相,甲醇-水为流动相梯度洗脱,以激发波长220 nm、发射波长312nm的荧光检测器进...     

Sensitive determination of cinnarizine in human plasma by high performance liquid chromatography and fluorescence detection

Summary A sensitive high performance liquid chromatographic method has been developed for the determination of cinnarizine in human plasma. Cinnarizine and clocinizine (internal standard) were extracted from acidified plasma (pH 4.7) into carbon tetrachloride and the organic layer was evaporated. The products were separated on a Microspher C18 (3 m) column, using a mixture of 0.04 % triethylamine in 0.01 M ammonium dihydrogen phosphate (NH₄H₂PO₄), pH adjusted to 4.2 with orthophosphoric acid (H₃PO₄), and acetonitrile (2080, v/v) as mobile phase, at a flow rate of 1 ml/min at 40°C. Fluorescence detection (_ex = 245 nm, _em = 310 nm) was used; the detection limit was 0.5 ng/ml under the conditions used, and the calibration curve linear in the concentration range evaluated (1–60 ng/ml). The assay has been used to measure cinnarizine concentrations in plasma after oral administration to volunteers.     

污水中脂肪胺荧光衍生物的高效液相色谱分离及质谱鉴定

利用新型荧光试剂1,2-苯并-3,4-二氢咔唑-9-异丙基氯甲酸酯(BCIC)作为柱前衍生化试剂,在乙腈中,以硼酸钠缓冲液(pH 9)为催化剂,40 ℃下衍生反应10 min后获得稳定的荧光产物.在Eclipse XDB-C8色谱柱上,通过梯度洗脱对12种游离脂肪胺进行了分离和在线质谱定性.激发和发射波长分别为λex=333 nm,λem=390 nm.采用大气压化学电离源(APCI)正离子模式,实现了污水中脂肪胺的定性及相应含量测定.脂肪胺的线性回归系数大于0.9996,检出限在10.57～37.83 fmol.     

Ionic liquid foam floatation coupled with ionic liquid dispersive liquid–liquid microextraction for the separation and determination of estrogens in water samples by high‐performance liquid chromatography with fluorescence detection

An ionic liquid foam floatation coupled with ionic liquid dispersive liquid–liquid microextraction method was proposed for the extraction and concentration of 17‐α‐estradiol, 17‐β‐estradiol‐benzoate, and quinestrol in environmental water samples by high‐performance liquid chromatography with fluorescence detection. 1‐Hexyl‐3‐methylimidazolium tetrafluoroborate was applied as foaming agent in the foam flotation process and dispersive solvent in microextraction. The introduction of the ion‐pairing and salting‐out agent NH₄PF₆ was beneficial to the improvement of recoveries for the hydrophobic ionic liquid phase and analytes. Parameters of the proposed method including concentration of 1‐hexyl‐3‐methylimidazolium tetrafluoroborate, flow rate of carrier gas, floatation time, types and concentration of ionic liquids, salt concentration in samples, extraction time, and centrifugation time were evaluated. The recoveries were between 98 and 105% with relative standard deviations lower than 7% for lake water and well water samples. The isolation of the target compounds from the water was found to be efficient, and the enrichment factors ranged from 4445 to 4632. This developing method is free of volatile organic solvents compared with regular extraction. Based on the unique properties of ionic liquids, the application of foam floatation, and dispersive liquid–liquid microextraction was widened.