Determination of zolpidem and zopiclone in serum by capillary column gas chromatography

A gas chromatographic method using a short, high-resolution capillary column connected to a specific thermoionic detector and requiring a simple and short extraction step without evaporation was developed for the rapid and precise determination of two new hypnotics, zolpidem and zopiclone, in serum at concentrations greater than 5 ng/mL. The assay was linear between 5 and 200 ng/mL, with coefficients of intra- and interassay variation less than 5% for both. The method was validated and then used to analyze zolpidem serum concentrations in nine rabbits after oral administration of 0.5 mg/kg and zopiclone serum concentrations in six patients treated orally with a 7.5-g dose.     

毛细管气相色谱法测定血清非洛地平浓度

采用毛细管气相色谱电子捕获检测器，以尼群地平为内标物质，对人血清中非洛地平的测定方法进行了初步的研究。实验结果，样品与内标的峰高比（Ｈｓ／Ｈｉ）同样品浓度间线性良好，线性范围０．５～４０ｎｇ·ｍｌ－１，回归方程Ｃ＝７．５７６Ｈｓ／Ｈｉ－０．０４３２，ｒ＝０．９９８９。最低检测限０．４ｎｇ·ｍｌ－１（信噪比３∶１）；精密度试验，日内误差ＲＳＤ＜６．３％，日间误差ＲＳＤ＜７．５％；方法平均回收率为８０．４％。结果显示，本法适于血清中非洛地平原形药物的测定。     

Determination of guaifenesin in human serum by capillary gas chromatography and electron capture detection

A method for the quantitation of guaifenesin in human serum has been developed and validated. The procedure involves liquid-liquid extraction of the serum sample in the presence of mephenesin as an internal standard, followed by derivatization and analysis using capillary gas chromatography (GC) and electron capture detection (ECD). Different solvents were tested for extraction of guaifenesin from serum. n-Hexane/dichloromethane (1:1, v/v) gave the highest recovery and the lowest background and was chosen as the extraction solvent. After extraction, the residue of guaifenesin was derivatized at 60 degrees C for 30 min, with trifluoroacetic acid anhydride (TFAA) in toluene in the presence of pyridine. Excess trifluoroacetic acid anhydride was removed using dilute solution of ammonium hydroxide. The method proved to be linear over the range of 25.0-1000 ng/ml. Recovery of guaifenesin from spiked samples was consistent, averaging 75.5% at 50.0 ng/ml with a range of 72.0-80.0% (N = 8 determinations) and averaging 78% at 800 ng/ml with a range of 76.0-81.0% (N = 8 determinations). The internal standard recovery was also consistent averaging 72.8% with a range of 67.0-76.0% (N = 16 determinations).     

Identification of polysaccharides in pharmaceuticals by capillary gas chromatography

A sensitive method for the identification of polysaccharides in pharmaceuticals is described. Polysaccharides are isolated by gel filtration and subsequently hydrolysed. The monomeric carbohydrates obtained are transformed into oxime-trimethylsilyl derivatives and analysed by capillary gas chromatography. Profiles of 13 different natural or semi-synthetic polysaccharides are discussed. The profiles of the hydrolysis products can be used to identify the polysaccharides mentioned above. Possible interferences by other polymers are given. The method can be used to identify most polysaccharides used as pharmaceutical adjuvants.     

毛细管气相色谱法测定化妆品中对羟基苯甲酸酯的含量

目的建立毛细管气相色谱法测定化妆品中的对羟基苯甲酸甲酯和对羟基苯甲酸乙酯。方法采用溶液直接进样法测定,DB-17毛细管柱,FID检测器,分流比10∶1。结果两种防腐剂在10～200μg·mL-1浓度范围内呈良好线性关系,相关系数分别为0.9992、0.9993,两种化合物的加标回收率为95%～98%。结论本法耗时少,分离度高,用标准曲线法测定,方法简单可靠。     

Determination of fluperlapine in human plasma by capillary gas chromatography

A sensitive and simple gas chromatographic method was developed for the determination of fluperlapine in human blood plasma using amitriptyline as an internal standard. The compounds were extracted into diethyl ether, the extract chromatographed on a dimethyl silicone capillary column, and detected by nitrogen phosphorus selective flame ionization detector. The NP-FID responses, as peak area ratios of the compound and internal standard, were linearly correlated to their plasma concentrations between 10 and 1000 ng/ml. The limit of detection in plasma was 0.5 ng/ml. The relative recovery of fluperlapine was about 85%.     

毛细管气相色谱法测定腺苷钴胺中有机溶剂残留量

目的建立腺苷钴胺中丙酮残留量的测定方法。方法采用直接进样毛细管气相色谱法,色谱柱为DB-624毛细管柱,载气为氮气,FID检测器,四氢呋喃为内标物,DMF为溶剂,测定了腺苷钴胺原料中丙酮的残留量。结果丙酮在5.0～45.0mg·L-1质量浓度范围内具有良好的线性,r=0.9998,检测限为0.1mg·L-1,平均回收率为101.1%。结论方法简便、灵敏,结果准确可靠,适用于腺苷钴胺中丙酮残留量的检测。     

毛细管气相色谱法测定丁硼乳膏中丁香酚的含量

目的 建立CGC法测定丁硼乳膏中丁香酚的含量.方法 采用毛细管气相色谱法测定,色谱柱为HP-5(0.32 mm×30 m,0.25μm)毛细管柱;程序升温,初始温度为60%,维持2 min后,以10℃·min-1升温至180℃;FID检测器;分流比5:1.结果 丁香酚进样量在1.4～700 ng范围内,丁香酚浓度与丁香酚峰和内标物峰面积之比值呈良好的线性关系,r=0.9999,平均回收率为96.5%,RSD为1.6%(n=6).结论 本法操作简便,结果准确,重现性好,为丁硼乳膏的质量控制提供可行的含量测定方法.     

毛细管气相色谱法测定糜蛋白酶中残留有机溶剂

目的建立测定糜蛋白酶中有机溶剂丙酮残留量的方法。方法采用毛细管气相色谱法，色谱柱为Supeleo 25301-U型石英毛细管柱，检测器为氢火焰离子化检测器，载气为高纯度氮气，水为溶解介质，检测了糜蛋白酶中丙酮的残留量。结果丙酮在样品中达到完全分离，在1．59—25．50ppm浓度范围内具有良好的线性，线性方程为A：306．0C＋184．3，r=0．9995，检测限为0．03ppm，方法回收率为99．9％，RSD为1．7％。结论本法能快速准确的检测糜蛋白酶中有机溶剂丙酮残留量，可用于糜蛋白酶质量控制中的有机残留溶剂检查。     

Determination of pethidine in rabbit plasma by capillary gas chromatography

A simple and fast gas chromatographic method for the determination of pethidine hydrochloride in rabbit plasma is described and validated. This method is an improvement on the GC method which uses a glass column, and was described previously by Koska et al. [Anaesth. Analg. 60 (1981) 8]. The samples were analysed by a GC 5890 HP system using Rtx-5, fused-silica capillary column linked to a nitrogen-phosphorus ionization detector. Lidocaine hydrochloride was used as the internal standard. Calibration curves were linear within the range 5-200 ng/ml. The limit of quantification was about 5 ng using a 1-ml biological sample and no interference was observed in the blank plasma. The mean recovery of the drug from plasma samples was 95.71+/-2.82%. This procedure turned out to be sensitive and convenient enough for the use in pharmacokinetic studies of pethidine.     

毛细管气相色谱法测定哌拉西林中残留溶剂

目的 建立气相色谱法分离测定哌拉西林中残留溶剂二氯甲烷、丙酮与乙酸乙酯.方法 以HP-624毛细管柱为色谱柱(30 m×0.53 mm×3.00 μm),载气为氮气,采用氢火焰离子化检测器,进样口温度为140℃,检测器温度为250℃,采用程序升温(60℃,保持12 min,以20℃·min-1升至240℃),采用顶空进样法,进样量1.0 ml.结果 在本色谱系统中,二氯甲烷、丙酮与乙酸乙酯互不干扰,分离度及检出灵敏度均符合要求,最小检出浓度分别为1.43,0.20,0.20 mg·L-1.结论 本方法可测定哌拉西林中残留溶剂量,方法简单、准确.     

毛细管气相色谱法测定撒烈痛片含量

本文采用毛细管气相色谱法测定撒烈痛片的含量。色谱柱：交联ＳＥ－５４弹性石英毛细管柱（０．２５ｍｍｉｄ×２５ｍ），氢火焰离子化检测器（ＦＩＤ），进样量在０．３ｍｇ－１．３ｍｇ内４种成分与峰面积比呈直线相关（非那西丁：ｙ＝２．９５５４ｘ－０．１２８１，ｒ＝０．９９９５；咖啡因：ｙ＝１．５５８４ｘ－０．０２５７，ｒ＝０．９９９４；氨基比林：ｙ＝１．１６５３ｘ－０．０８９３，ｒ＝０．９９９２；苯巴比妥：ｙ＝２．５３５ｘ－０．１７５４，ｒ＝０．９９９８）。平均回收率±标准差分别为１００．２％±１．１７％、９９．８％±１．９４％、１００．５％±１．４６％、９８．４％±１．８２％。     

毛细管气相色谱法测定阿奇霉素中的丙酮残留量

目的建立阿奇霉素中丙酮残留量的测定方法。方法采用毛细管气相色谱法,氢火焰离子化检测器(F ID),以N,N-二甲基甲酰胺(DM F)为溶剂,弹性石英毛细管柱DB-624(30m×0.53mm,3μm);柱温40℃维持10m in,以40℃/m in的速率升温至200℃,维持10m in;载气:高纯氮气,线速度4m l/m in;氢气:40m l/m in;进样口温度250℃;检测口温度280℃;空气400m l/m in;尾吹25m l/m in;分流比2∶1;进样量1μl。结果加样回收率为99.84%,RSD为0.87%。结论本法简便、灵敏、专属、准确,毒性小。     

毛细管色谱法测定洛美沙星中的有机溶剂残留量

目的：建立毛细管气相色谱法测定洛美沙星中的有机溶剂残留量。方法：用INNOWAX毛细管气相色谱柱，FID检测器，以2-戊酮为内标进行测定。结果：乙酸乙酯、四氢呋喃、乙醇、乙腈的线性范围分别为0～80μg／ml(r=0．9997)、0～11．52μg／ml(r=0．9996)、0～80μg／ml(r=0．9997)，0～6．56μg／ml(r=0．9996)；平均回收率分别为100．5％、100．1％、101．2％、100．1％；RSD分别为1．30％、0．9％、1．18％和1．23％(n=9)。结论：本方法简单、准确、灵敏度高、重现性好，适用于洛美沙星中有机溶剂残留量的测定。     

毛细管法测定莫西沙星中的有机溶剂残留量

目的建立毛细管气相色谱法测定莫西沙星中的有机溶剂残留量。方法用INNOWAX毛细管气相色谱柱,FID检测器,以乙腈为内标进行测定。结果乙醚、甲醇、N,N-二甲基甲酰胺(DMF)的线性范围分别为50～800μg/mL(r=0.9998)、30～480μg/mL(r=0.9999)、8.8～140.8μg/mL(r=0.9996);乙醚、甲醇、DMF的平均回收率分别为99.71%、100.3%、99.54%;RSD分别为1.87%、1.32%、1.67%(n=9)。结论该方法简单、灵敏、准确、重现性好,适用于莫西沙星中的有机溶剂残留量的测定。     

毛细管气相色谱法测定角鲨烯软胶囊中角鲨烯的含量

目的 建立毛细管气相色谱法测定角鲨烯软胶囊中角鲨烯的含量.方法 采用毛细管气相色谱法;色谱柱为RTX-5弹性石英毛细管柱(30 m×0.32 mm,0.25 μm);载气为氮气;检测器为FID;进样口和检测器温度均为280℃;柱温为250℃.结果 角鲨烯在1～50 mg·L-1与峰面积线性关系良好,r=0.997 6;加样回收率平均为100.8％(n=9);检测限为0.4 ng;定量限为2ng.结论 本法灵敏度高,简单易行,结果准确可靠,可为角鲨烯的质量控制提供依据.     

毛细管气相色谱法测定头孢米诺钠中几种有机溶剂残留量

目的:建立头孢米诺钠中几种有机溶剂残留量的测定方法.方法:采用毛细管气相色谱法,色谱柱为PEG-20M石英毛细管柱(30 m×0.53 mm,1.2μm),程序升温技术,用内标对比法分离测定头孢米诺钠中的残留溶剂.结果:建立的色谱方法对待测溶剂具有良好的分离度,在所考察的浓度范围内线性关系良好,各溶剂回收率在98.2%～100.4%,检测限1～3 ng.结论:该方法灵敏度、准确度均达到有机溶剂残留量的检测要求,可用于头孢米诺钠中残留有机溶剂的检测.     

毛细管气相色谱法测定甲磺酸罗哌卡因中的有机溶剂残留量

目的建立气相色谱法测定甲磺酸罗哌卡因原料药中2种有机溶剂残留量的方法。方法以2%二甲亚砜水溶液为溶剂溶解样品,直接进样,在DB-624(30.0 m×320μm×1.8μm)毛细管柱上程序升温,应用FID检测器,载气为氮气。结果 N,N-二甲基甲酰胺与甲苯均能得到有效分离,各组分在考察的浓度范围内线性关系良好,r=0.9997~0.9999,平均回收率为96.2%~102.2%。结论该方法可用于检测甲磺酸罗哌卡因原料药中N,N-二甲基甲酰胺与甲苯的残留量。     

毛细管气相色谱法测定替格瑞洛中溶剂残留量

目的建立毛细管气相色谱法测定替格瑞洛中7种有机溶剂残留量。方法采用DB-624色谱柱(60 m×0.53 mm,3.0μm),氮气作为载气,采用氢火焰离子化检测器检测,以N,N-二甲基甲酰胺为溶剂,以正己烷为内标物,检测替格瑞洛原料药中残留溶剂。结果二氯甲烷、甲醇、乙酸乙酯、四氢呋喃、正庚烷、乙醇和醋酸线性关系良好(r=0.999 0~0.999 6),平均回收率为99.0%~101.1%,定量限分别为4.23、3.00、2.50、1.44、1.00、2.00和5.01 mg·L~(-1)。结论建立的方法适用于替格瑞洛中7种残留溶剂的同时测定。