共查询到19条相似文献，搜索用时 234 毫秒
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采用HPLC法测定了普鲁卡因青霉素注射液中青霉素的含量.色谱柱为spherisorb ODS/5 μm(250 mm×4.6 nm),流动相为缓冲液-水-乙腈(5223 25,V/V),检测波长235 nm,流速1.65 mL/min,柱温30 ℃.在0.16～1.6 mg/mL的浓度范围内青霉素的峰面积与浓度呈良好线性关系(r=0.999 2),平均回收率100.2%,RSD为0.5%.该方法适用于检测普鲁卡因青霉素注射液.与微生物法相比,该方法具有准确、简便、快速等优点. 相似文献
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建立了普鲁卡因青霉素注射液鉴别和含量测定的HPLC方法。样品经HPLC分离后进行定性鉴别和含量测定。结果显示供试品溶液主峰的保留时间与对照品溶液主峰的保留时间一致,普鲁卡因的线性范围为0.432-0.648 mg/mL,青霉素的线性范围为0.64-0.96 mg/mL,普鲁卡因和青霉素的添加回收率分别为101.35%和100.11%。该方法结果准确度高、精密度好,可作为质量标准控制方法。 相似文献
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应用反相高效液相色谱法(RP-HPLC)测定复方布他磷注射液中布他磷的含量,采用C8色谱柱(4.6 mm×250 mm,粒度:5μm),以甲醇:0.1%磷酸水溶液(10∶90,V∶V)为流动相,流速1 ml/min,示差折光检测器检测。该反相高效液相色谱法测定的布他磷浓度在0.64~0.96 mg/mL范围内有良好的线性关系;回归系数r2=0.9992;样品溶液至少在24 h内稳定(RSD=0.13%);进样精密度(RSD=0.18%)良好;高、中和低三种浓度下布他磷的回收率均大于99%(RSD<1.0%),回收率良好。本法简便、快速、准确,可用于复方布他磷注射液中布他磷含量的测定。 相似文献
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UPLC和HPLC法检测猪肉中磺胺类药物残留的比较 总被引：1，自引：0，他引：1
比较了超高效液相色谱法与高效液相色谱法测定猪肉中磺胺类药物残留的结果。采用农牧发[2001]38号动物源食品中磺胺类药物残留的检测方法有关标准,将原高效液相色谱方法转换并优化为超高效液相色谱方法。高效液相色谱方法色谱柱为Waters Symmetry C18柱(4.6 mm×250 mm,5μm),流动相:乙腈-甲醇-水-乙酸(2∶2∶9∶0.2),流速:1 mL/min,进样量:50μL;超高效液相色谱方法色谱柱为Waters Acquity UPLC BEH RP18柱(2.1 mm×50 mm,1.7μm),流动相:乙腈-甲醇-水-乙酸(2∶2∶10∶0.2),流速:0.4 mL/min,进样量:5μL。结果表明超高效液相色谱方法能够替代高效液相色谱分析方法测定猪肉中磺胺类药物残留,既加快了分析速度,达到了样品分析的高通量,减少有机溶剂的使用,又得到更高的分析灵敏度。 相似文献
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完善甜瓜蒂质量标准并提高。采用薄层色谱法对甜瓜蒂进行定性鉴别,并采用高效液相色谱法测定葫芦素B的含量,色谱条件:Agilent HC-C18色谱柱(250 mm×4.6 mm,5μm),乙腈-0.1%磷酸溶液(60∶40)为流动相,流速为1.0 mL/min;检测波长为228 nm。结果表明,薄层色谱斑点清晰,分离度好,专属性强,重复性良好;高效液相色谱法测定葫芦素B的回归方程为:Y=1 367 962.09X+465.59,r=0.999 6,在0.0340~4.247 0 mg/mL线性关系良好;平均回收率为98.4%,RSD为1.6%。说明该研究建立的薄层色谱鉴别和高效液相色谱含量测定方法简便、快捷、结果准确、可靠,为甜瓜蒂质量标准的修订完善提供了可靠依据。 相似文献
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采用高效液相色谱法测定胆翘注射液中黄芩苷的含量[1]。色谱柱为Agilent Eclipse XDB-C18(5μm,250mm×4.6mm id),流动相为甲醇—水—冰乙酸(50∶50∶1),检测波长为274nm,流速1.0mL/min,柱温30℃。在相同的色谱条件下,探讨50%甲醇溶剂、流动相(50∶50∶1)对含量测定的影响,实验结果表明,不干扰黄芩苷含量结果测定(见图1、图2)。黄芩苷在0-100μg/mL浓度范围内线性关系良好R2=0.9999(n=6),回归方程为y=19.7840X+4.9103,回收率为97.6%~98.9%,相对标准偏差为0.5%。本方法简单、准确、可行,适用于胆翘注射液中黄芩苷含量测定。 相似文献
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建立了用固相萃取-高效液相色谱法(HPLC)测定鸡粪便中洛克沙胂(ROX)的方法。鸡粪便采用0.05 mol/L磷酸氢二钾∶甲醇=90∶10(V/V)溶液作提取液,用Waters Oasis(MAX固相萃取小柱净化;色谱条件为:Agilent C18色谱柱(4.6×250 mm,5μm),流动相为0.05 mol/L磷酸二氢钾∶100 mL/L乙酸∶甲醇=90∶7∶3(V/V/V),流速1.0 mL/min,柱温30℃,进样量20μL,紫外检测波长266 nm。ROX的浓度在10.0μg/mL范围内,线性相关系数为0.999 9,方法的回收率为80.09%～81.5%,变异系数为2.09%～5.87%,检出限为1.0 mg/kg。该方法精确度和灵敏度很高,适用于鸡粪便中ROX含量的测定。从某鸡场随机采集8个粪样,调查鸡粪中的ROX含量,其ROX的平均浓度为21.49 mg/kg。 相似文献
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采用高效液相色谱法,以C18为色谱柱,以甲醇∶水(25∶75)为流动相,检测波长为250 nm,测定葛根中葛根素的含量.结果表明,葛根中葛根素的含量在20～140 μg/mL,线性关系良好(r=0.9999).平均回收率97.40%,RSD=3.0%.本方法测定简便、快速、测定结果准确. 相似文献
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建立一种超高效液相色谱法测定饲料中硝西泮含量的方法。样品经无水乙醇提取,定容,采用超高效液相色谱分离,PDA检测器检测,以保留时间定性,以峰面积定量。硝西泮在浓度0.1~20μg/mL范围内线性良好,相关系数r为1.0000。在2~100mg/kg添加浓度范围内,回收率为81.6%～105.6%,批内RSD为3.8%～7.0%,批间RSD为0.9%～1.7%。最低检测限为2mg/kg,定量限为4mg/kg。该方法操作简便、结果准确、稳定性好,适用于饲料中硝西泮的测定。 相似文献
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超高效液相色谱法测定鳗鱼中氟乐灵残留量 总被引：1，自引：0，他引：1
建立了一种超高效液相色谱法测定鳗鱼中氟乐灵残留量的方法.样品经正己烷均质提取,浓缩后经弗罗里硅土小柱净化,浓缩,甲醇定容,超高效液相色谱分离,TUV检测器检测,以保留时间定性,以峰面积定量.结果表明:在0.05～5μg/mL范围内浓度与峰面积线性关系良好,相关系数r=0.999 97;在0.01～0.5 mg/kg添加... 相似文献
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鱼腥草注射液中非法添加水杨酸和氧氟沙星HPLC-PDA检测方法的建立 总被引：2，自引：2，他引：0
为建立鱼腥草注射液中非法添加水杨酸和氧氟沙星的测定方法,采用十八烷基键合硅胶为填充剂,磷酸二氢钠溶液(取磷酸二氢钠3.0 g,加1000 m L水使溶解,加三乙胺0.5 m L,用氢氧化钠饱和溶液调节p H值至7.0)-甲醇为流动相,梯度洗脱,流速为1.0 m L/min,二极管阵列检测器,提取波长为293 nm。采用峰纯度检查和光谱相似度检查辅助对照品比对方法,对非法添加药物进行确证。在此液相色谱条件下,水杨酸、氧氟沙星与其他物质峰分离良好。按外标法以峰面积计算,水杨酸和氧氟沙星的平均回收率分别为99.3%和98.8%,RSD分别为0.6%和0.8%。结果表明该检测方法简便、准确、可靠,可用于同时测定鱼腥草注射液中非法添加的水杨酸和氧氟沙星。 相似文献
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目前,国标法-气相色谱法中测定食品中肌醇含量的方法存在操作步骤繁琐,操作稳定性不高,检测时间长的不足,为此,本文对《GB 5009.270—2016食品安全国家标准食品中肌醇的测定》中的气相色谱法进行了试样前处理、标品配制、色谱条件的优化.试验结果表明,本方法在0.02～0.12 mg范围内,呈良好的线性关系,相关系数... 相似文献
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建立了高效液相色谱法(HPLC)测定兽用除虫脲原料药含量及有关杂质的检测方法。采用C18色谱柱(250 mm×4.6 mm,5μm),以甲醇为流动相A,0.01 mol/L乙酸铵溶液为流动相B,进行梯度洗脱,流速1.0 mL/min,检测波长254 nm,进样量10μL,柱温25℃。除虫脲的线性范围为10~1000μg/mL(R 2=0.999),回收率97.01%~100.83%(RSD<1.0%,n=3),精密度(RSD=0.13%,n=9)、重复性(RSD=0.45%,n=6)良好,主成分与各杂质峰分离良好。以主成分自身对照法计算,各杂质峰面积的和不得大于对照溶液主峰面积的0.1倍(0.1%)。该方法简便灵敏,结果准确可靠,可作兽用除虫脲原料药含量及有关杂质测定。 相似文献
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A Franklin M Horn af Rantzien N Obel K Ostensson G Astr?m 《American journal of veterinary research》1986,47(4):804-807
Concentrations of benzylpenicillin and spiramycin adipate were determined in bovine plasma and milk and in lymph draining the udder tissue after IM or IV administration. Combined benzylpenicillin and dihydrostreptomycin sulfate concentrations were also determined in the same fluids after intramammary injection. A superficial parenchymal lymph vessel, afferent to the supramammary lymph gland of the left quarters, was cannulated with a polythene catheter from which the lymph was allowed to drain freely. After injections of 9.5 mg of benzylpenicillin/kg of body weight IM, a mean peak concentration (PC) in lymph (3.7 micrograms/ml), constituting 77% of the PC in plasma (4.8 micrograms/ml), was obtained 0.5 to 1 hour after PC in the plasma. The benzylpenicillin lymph concentration was close to that in plasma for about 7 hours after injection. Thereafter, the benzylpenicillin lymph concentration continued to exceed that in plasma, but not that in milk. After IV administration of spiramycin adipate, the lymph concentration was almost identical to that in plasma. After intramammary injection of procaine benzylpenicillin (400 mg), in combination with the same amount of dihydrostreptomycin sulfate, into 2 udder quarters each, mean PC in the lymph of 3.5 micrograms/ml and 8.4 micrograms/ml, respectively, were obtained 6 hours after injection. In plasma, the mean PC of benzylpenicillin (0.07 micrograms/ml) and of dihydrostreptomycin sulfate (0.85 micrograms/ml) were obtained after 4 and 6 hours, respectively. In milk from the nontreated quarters, a mean concentration of 5 ng of benzylpenicillin/ml was obtained, whereas dihydrostreptomycin sulfate (greater than or equal to 0.3 microgram/ml) was not detected.(ABSTRACT TRUNCATED AT 250 WORDS) 相似文献
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建立了帕那珠利原料药含量测定的HPLC法.以0.2％乙酸水溶液-乙腈(43∶57)为流动相,采用Diamonsil C18反相色谱柱(250 mm×4.6 mm,5μm),柱温35℃,流速1 mL/min,紫外检测波长255 nm.在此实验条件下,帕那珠利在10 ～ 100 μg/mL浓度范围内与峰面积线性关系良好(r=0.9999,n=5);精密度良好,RSD为0.25％(n=5);平均回收率为98.6％,RSD为1.2％.(n=9);重现性良好,RSD为0.69％(n=5);样品在24h内稳定,RSD为0.74％.本方法准确、简便、快速,可以用于帕那珠利的含量测定. 相似文献
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Olsén L Ingvast-Larsson C Broström H Larsson P Tjälve H 《Journal of veterinary pharmacology and therapeutics》2007,30(3):201-207
Case reports of 59 horses reacting adversely to procaine benzylpenicillin or to sodium or potassium benzylpenicillin in Sweden in 2003-2005 were obtained through contacts with horse-owners. For the assessment of the reports, various parameters were evaluated, such as the times to the reactions, information on previous penicillin treatment, the clinical signs and the actions taken in the reacting horses. Among the reports, two horses had received sodium or potassium benzylpenicillin intravenously, whereas the remaining 57 horses had been treated with procaine benzylpenicillin intramuscularly. Allergy may underlie the adverse reactions in the horses given sodium and potassium benzylpenicillin, and in a few of the horses given procaine benzylpenicillin. However, in most horses in the latter group, the clinical signs may be due to the toxic effects of procaine. In these horses, the dominating clinical signs were locomotor and behavioral changes. Some risk factors may enhance the probability that horses react to procaine. One is repeated injections, which increase the likelihood of intravascular administration and also may increase the sensitivity to procaine due to neuronal sensitization (kindling). Procaine is rapidly hydrolyzed by plasma esterases to nontoxic metabolites. When high amounts of procaine enter the circulation, the hydrolyzing capacity may be exceeded and toxicity occurs. Analyses of plasma esterases from reacting horses showed lower activity than in nonreacting control horses. Low esterase activity may increase the possibility of procaine toxicity and constitute another risk factor. 相似文献
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HPLC-PDA法同时测定黄芪多糖注射液中非法添加的四种解热镇痛类药物 总被引：3，自引：3，他引：0
采用迪马钻石C18(250 mm×4.6 mm,5μm)柱,以磷酸盐缓冲液(磷酸二氢钠6.0g,加水1000 mL使溶解,加三乙胺1mL,用氢氧化钠试液调pH值至7.0)-甲醇(70∶30,V/V)为流动相,流速1.0 mL/min,建立了同时测定黄芪多糖注射液中非法添加四种解热镇痛类药物的HPLC-PDA法.结果显示,在该色谱条件下四种解热镇痛类药物得到良好分离,在测定范围内线性关系良好,检测限1 ～4 μg/mL,定量限5～10 μg/mL,回收率均大于99.0％.本方法简便、灵敏、准确、快速、重现性好,可对黄芪多糖注射液中非法添加的四种解热镇痛类违禁药物进行定性和定量检测. 相似文献