Quick valence analysis method of vanadium toward accurate toxicity assessment of vanadium-containing hazardous wastes

In order to develop a quick, efficient and sensitive valence analysis method of vanadium(V), the high- performance liquid chromatography (HPLC) was utilized to separate and quantify EDTA-complexed V(III), V(IV) and V(V) ions. The influence of EDTA, TBAOH, solution pH and organic modifier on retention behavior of V−EDTA complexes was investigated. Complexed V(III), V(IV) and V(V) ions can be separated and quantified in 5 min, with detection limits of 0.04 mg/L V(III), 0.07 mg/L V(IV), and 0.06 mg/L V(V), respectively. The established method is applied to analyzing the hazardous waste of V−Cr-bearing reducing slag and results demonstrate 49.94% of its V element to be toxic V(V). This work opens a new avenue for quick and accurate toxicity assessment of hazardous wastes containing multivalent heavy metals.     

HPLC-UV法测定微生物降解体系中3-苯氧基苯甲酸含量

采用高效液相色谱-紫外(high-performance liquid chromatography with ultraviolet,HPLC-UV)法测定微生物降解体系中3-苯氧基苯甲酸(3-PBA)的含量。以Gemini 100A C18柱(150mm×4.60mm,5.0μm)为色谱柱,乙腈-水(70:30,V/V)为流动相,流速0.7mL/min,用紫外检测器在210nm处检测3-PBA。结果显示：3-PBA对照品的保留时间为4.268min,线性范围为0.5～50.0mg/L,3-PBA平均回收率为98.919%,RSD为2.78%;运用该方法测得4种不同来源的混合菌株发酵液中3-PBA的残留量分别为24.467、86.266、2.633、1.921mg/L。本法简单、快速、准确、分离度好。     

HPLC-UV法检测土壤中的3-硝基苯并蒽酮

建立了HPLC-UV法检测土壤中多环芳烃类物质3-硝基苯并蒽酮的方法.采用on UltimateXB-C18（5μm,150mm×4.6mm i.d.）柱,流动相为甲醇∶水=7∶3（v/v）,流速为0.5mL/min,柱温为30℃,检测波长为391nm.在此色谱条件下,3-硝基苯并蒽酮在0.2～40μg/mL范围内具有良好的线性关系,最低浓度检测限为78ng/mL（S/N=3）.利用超声波萃法对土壤中的3-硝基苯并蒽酮进行了萃取,并用HPLC-UV法测出了其含量.     

高效液相色谱法定量尿酸、黄嘌呤和次黄嘌呤在人体血清中的浓度

目的: 建立高效液相色谱法测定尿酸、黄嘌呤和次黄嘌呤在人体血清中的浓度。方法: 用Agilent ZORBAX SB-Aq column色谱柱,ZORBAX-Extend C₁₈预柱,以甲醇和 47 mmol/L KH₂PO₄水溶液作为流动相,流速:1.0 mL/min,检测波长为 260 nm。结果: 血清中尿酸、黄嘌呤和次黄嘌呤的线性范围分别是(1.667~166.667)×10³ ng/mL (r=0.9995)、(0.033~3.338)×10³ ng/mL(r=0.9994)和 (0.033~3.338)×10³ ng/mL (r=0.9996),日间与日内精密度均<15%。结论: 该法灵敏度高,精密度和准确度佳,能满足非布司他体内药效学研究。     

高效液相色谱—紫外检测法测定微生物降解体系中己烯雌酚含量

采用HPLC—UV法测定微生物降解体系中己烯雌酚(DES)的含量。根据霉菌和细菌发酵体系的不同性质选用不同的提取方法,以Sepax GP-C18柱(150 mm×4.60 mm,5.0μm)为色谱柱,甲醇:水(7:3,V/V)为流动相,流速0.7mL/min,用紫外检测器在242nm处检测。结果显示DES对照品的保留时间为7.714min,在0.5~50.0mg/L浓度范围内线性关系良好,相关系数为0.996 3。细菌发酵液中DES平均回收率为94.04%,RSD为2.33%;霉菌发酵液中DES平均回收率为95.24%,RSD为1.05%。DES的检出限不大于0.30mg/L。运用该方法测得实验室保藏的4株菌5d内对25 mg/L的DES降解率分别为62.38%,64.72%,53.38%,88.34%。该方法检测微生物降解体系中DES简单、快速、准确、分离度好,精密度高,稳定性好。     

α-与β-甘草酸在小鼠体内分布的研究

目的 探讨甘草酸(glycyrrhizic acid, GL) 的两个差向异构体α-GL 和β-GL 在小鼠体内的分布及其特征。 方法 运用HPLC-UV 法检测小鼠单次iv α-GL 或β-GL 53 mg·kg^-1后5、15、30、60 和180 min 时体内各组织脏器中的药物含量, 比较、评价两者的分布差异及特征。 结果 α-GL 和β-GL iv 后分布迅速,除血外, 肝中含量最高, 肺、肾、脂肪、心、卵巢、肠、脾、睾丸、肌肉中药物含量依次减小, 脑中最低;肠肝循环的第二峰现象出现在30 min 时;α-GL iv 后早期肝含量显著高于β-GL, 血及其余组织脏器药物含量明显低于β-GL 或与其相近;随时间的延长药物含量迅速降低的同时肠浓度渐高, 至180 min 时α-GL 各组织脏器(除肠外) 药物浓度接近或低于检测限, β-GL 则仍维持较高浓度, 是峰值的30 %~ 70 %。 结论 小鼠iv α-GL 后在体内呈肝分布特异性, 转化成GA 的速率高于β-GL, 无组织蓄积;而β-GL 在体内分布广泛, 代谢较慢, 有蓄积的可能。     

Validation of an analytical method for the determination of carbadox and olaquindox in feedstuff by liquid chromatography coupled to UV and/or diode array detection

The performance characteristics of an analytical method based on high-performance liquid chromatography (HPLC) for the detection of the banned growth promoters, carbadox and olaquindox, in feedstuff were determined via a collaborative study. The relative standard deviation of repeatability (RSD_r) ranged 1.1-5.5% for carbadox and 2.5-6.2% for olaquindox. The relative standard deviation of reproducibility (RSD_R) ranged 6.4-10.7% for carbadox and 12.8-20.0% for olaquindox. In all cases, the HORRAT values were equal or below the critical value of 1.5. Moreover, trueness in all cases was between the acceptance limits of 80 and 110%. Consequently, it was concluded that the method is suitable for quantitative evaluation. The method was also qualitatively assessed in terms of correct identification of the target analytes by examination of the UV spectrum when the more specific diode array detector was coupled to HPLC. In all cases, the percentage of correct identifications was ≥94% for olaquindox and carbadox, while the percentage of false negatives was ≤6%, suggesting the extended utilization of the HPLC method from quantitative to confirmatory status with a diode array detector.     

刺五加叶的HPLC-UV和ESI-MS指纹图谱研究

对12批不同来源的刺五加叶提取物进行指纹图谱研究,并利用ESI-MS指纹图谱鉴别刺五加叶与山楂叶。分别采用高效液相色谱（HPLC-UV）和电喷雾电离质谱（ESI-MS）测定12批不同来源的刺五加叶提取物,利用ESI-MS技术测定刺五加叶与山楂叶提取物,得到了分离度、精密度和重现性均较好的刺五加叶HPLC-UV及ESI-MS指纹图谱;同时,利用刺五加叶与山楂叶ESI-MS指纹图谱的差异,成功鉴别了二者,可为刺五加叶药材的质量控制提供参考。     

Sorbate and benzoate in Turkish retail foodstuffs

From 2008 to 2011, surveys were conducted to determine the levels of benzoic and sorbic acids and their respective salts in 983 retail food samples which included sauces, vegetable and fruit preparations, flavoured syrups, food supplements, cereals, bakery products, jelly, synthetic cream, sprays, mustards, jam and preserves, molasses, chewing gum, confectionery, non-alcoholic beverages, tea, wine, vinegar, brine and beers. The analysis involved methanol extraction of the foodstuff and direct determination by HPLC with UV detection. Quality assurance was employed with each batch of samples. Accuracy was ensured through regular participation in proficiency tests. Over this four-year period, a total of 23 samples (2.3%), some syrups, tomato sauces and fruit contained individual or combined levels of sorbic and benzoic acids above regulatory limits. Unauthorised use of benzoic acid was also detected in a syrup sample, bakery products and fruit preserves.