母乳中甲硝唑药物代谢动力学的毛细管电泳研究

用毛细管电泳测定了甲硝唑在母乳中的含量,研究了其药代动力学。以液－液萃取作为样品预处理手段,萃取回收率在９０％～１０１％范围内。以替硝唑作为内标,采用场放大进样。该法在甲硝唑质量浓度为０．４０～２５．６７ｍｇ／Ｌ时,甲硝唑质量浓度和甲硝唑与替硝唑的峰面积之比呈线性,线性相关系数（ｒ）大于０．９９９,最低检测量为０．４０ｍｇ／Ｌ,检出限（Ｓ／Ｎ＝３）为０．１５ｍｇ／Ｌ,相对峰面积的相对标准偏差为１．     

高效液相色谱法测定大鼠血浆中氯解磷定含量及药代动力学研究

建立了高效液相色谱法（HPLC）测定血浆中氯解磷定（PAM）的含量,研究了不同给药方式对大鼠体内药代动力学行为的影响。优化条件为：色谱柱CAPCELL PAK C18 MGⅢ(250 mm×4.6 mm, 5μm),以5 mmol/L正庚烷磺酸钠溶液（含体积比0.12%三氟乙酸）-乙腈为流动相进行梯度洗脱,流速1 mL/min,检测波长294 nm,内标双复磷。血浆中PAM浓度在0.5～100 mg/L范围内与PAM和内标峰面积之比具有良好的线性关系,相关系数为0.9996。方法日内精密度分别为7.1%, 3.3%, 3.6%,日间精密度分别为9.1%, 9.7%, 7.1%,重复性相对标准偏差（RSD）为0.76%,可用于血浆中PAM的含量测定。药代动力学结果表明,相比静脉注射组,肌内注射组药物半衰期和平均滞留时间延长。肌内注射PAM更适用于急性中、重度有机磷中毒的临床治疗。     

硫普罗宁的药代动力学及光度法测定

建立了光度法测定硫普罗宁的新方法。研究表明:在SCN-和KNO3存在下,控制溶液pH4.0,Cu(II)被硫普罗宁还原生成的Cu(I)与SCN-反应形成CuSCN沉淀,该沉淀能浮在水相表面。通过测定溶液中剩余Cu(II)的量,可以测定硫普罗宁的含量。吸光度与硫普罗宁浓度之间存在良好线性关系。线性方程:A=4.898-0.3616ρ(μg/mL),线性范围为0.25～12.0μg/mL,相关系数R=0.9993,检出限为0.16μg/mL。该方法可直接用于药物中硫普罗宁含量的测定及其药代动力学行为研究。     

血浆中辛伐他汀分析方法及药代动力学研究

采用ＧＣ／ＭＳ的ＳＩＭ定量模式,以洛伐他汀做内标,经乙酸乙酯萃取后,测定人体血中辛伐他汀的浓度。标准曲线在０．２７－５４μｇ／Ｌ之间呈良好的线性关系,ｒ〉０．９９９,高中低３个浓度点的日间日内ＲＳＤ小于５．２％,回收率可达９６％－１０３％〈并应用在１０例健康志愿者口服４０ｍｇ辛伐他汀的药代动力学的研究。     

气相色谱法测定溴己新血药浓度及药代动力学研究

 建立了人血浆中溴己新的气相色谱 电子捕获测定法 ,对溴己新胶囊在健康人体内的药代动力学进行了研究。色谱柱为 5 %SE 30 (2m× 3mmi.d .)硅烷化玻璃柱。 5 氯 2 氨基二苯甲酮为内标 ,血浆样品加入磷酸盐缓冲液 (pH 6 0 )后用正己烷 二氯甲烷 (体积比为 9∶1)提取。线性范围为 1 0 μg/L～ 5 0 0 μg/L ,r =0 9994。人血浆中最小检测质量浓度为 0 5 μg/L。方法重现性好 ,日内、日间RSD分别小于 4 5 6 %和 7 11% ,平均回收率 97 5 %。 8名健康志愿者口服 8mg溴己新胶囊后 ,其体内代谢过程符合一房室模型。     

气相色谱法测定溴己新血药浓度及药代动力学研究

建立了人血浆中溴己新的气相色谱 电子捕获测定法 ,对溴己新胶囊在健康人体内的药代动力学进行了研究。色谱柱为 5 %SE 30 (2m× 3mmi.d .)硅烷化玻璃柱。 5 氯 2 氨基二苯甲酮为内标 ,血浆样品加入磷酸盐缓冲液 (pH 6 0 )后用正己烷 二氯甲烷 (体积比为 9∶1)提取。线性范围为 1 0 μg/L～ 5 0 0 μg/L ,r =0 9994。人血浆中最小检测质量浓度为 0 5 μg/L。方法重现性好 ,日内、日间RSD分别小于 4 5 6 %和 7 11% ,平均回收率 97 5 %。 8名健康志愿者口服 8mg溴己新胶囊后 ,其体内代谢过程符合一房室模型。方法可用于体内血药浓度测定 ,简单、快速 ,灵敏度高 ,数据准确可靠     

前列泰片在家兔体内的药代动力学研究

应用柱前衍生化HPLC法测定了以 4 %前列泰片悬浮液灌饲 (31mL/kg)家兔后 ,兔血浆中水苏碱 (Stachy drine)浓度 .结果表明水苏碱在家兔血中的经时变化符合二室模型 :峰浓度 (Cmax) 6 .2 9± 0 .84 μg/mL ;达峰时间(Tmax) 3.36± 0 .6 4h ;分布相半衰期 (T1/ 2α) 5 .35± 3.79h ;消除相半衰期 (T1/ 2 β) 32 .38± 2 4 .33h ;药时曲线下面积 (AUC)2 0 8.15± 118.4 μg/ (mL·h)     

有机锗—M10在兔体内的药代动力学研究

本文报道给每公斤体重的家兔以１６ｍｇ锗灌胃，定时采血，用三元络合荧光法监测不同时间的血药浓度，经计算机进行数据处理，得到了系列药代动力学参数，效果良好。     

RP/HPLC测定吡虫啉血药浓度及其大鼠灌胃药代动力学评价

建立了大鼠血浆中吡虫啉的反相高效液相色谱(RP/HPLC)分析方法,并用于吡虫啉在大鼠体内的代谢动力学行为及特征研究。血浆样品经甲醇萃取,反相HPLC法测定血浆中的吡虫啉浓度。色谱柱为Agilent ZORBAX C18柱(4. 6 mm×250 mm,5μm),流动相为甲醇-水(30∶70),进样量20μL,检测波长245nm,流速1. 0 m L/min。在最佳条件下,吡虫啉的线性范围为0. 5～100 mg·L-1(r2=0. 999 8),检出限为10μg·L-1,平均加标回收率为74. 7%。大鼠单剂量灌胃给予68. 1 mg·kg-1吡虫啉,分别测定给药后不同时间下血浆中吡虫啉的浓度,并计算代谢动力学参数。灌胃给药后吡虫啉的Cmax为23. 557 mg/L,tmax为7. 333h,t1/2α为4. 472 h,AUC(0-t)为276. 727 mg·h/L。代谢动力学结果显示,吡虫啉在大鼠体内呈二隔室模型分布,以一级药代动力学方式消除。该方法简便可靠,能够满足血浆中吡虫啉测定及药代动力学研究的要求。     

茶叶中咖啡因的纸基质室温Lin光法体内药代动力学研究

以快速定量滤纸为基质，用KL—NaAc为重原子微扰剂建立了测定痕量咖啡因的滤纸基质室温Lin光(PS-RTP)分析法。并用于茶叶中咖啡因的测定及其在人体内的药代动力学研究。实验表明：PS-RTP法用于茶叶中咖啡因的测定准确、灵敏。受试者饮茶后1-2h尿样中咖啡因排泄达高峰，24h后基本排泄完毕。咖啡因的尿排泄量占总摄取量的64．25％。     

母乳中多种含卤持久性有机污染物的联合检测方法

建立了母乳中多种含卤持久性有机污染物(POPs)的联合检测方法,目标化合物主要包括六溴环十二烷(HBCDs)、多溴联苯醚(PBDEs)、多氯联苯(PCBs)和有机氯农药(OCPs)等.样品的前处理采用液液萃取、凝胶渗透色谱(GPC)净化和固相萃取(SPE)等技术,目标化合物经气相色谱-质谱联用仪(GC-MS)、液相色谱-三重四极杆串联质谱联用仪(LC-MS/MS)和气相色谱-三重四极杆串联质谱联用仪(GC-MS/MS)等进行检测.样品通过GPC除去脂肪,然后经SPE柱进一步净化并进行多组分分离,极大程度地减小了生物样品中复杂基质的干扰,适合样品量相对较小的人体样本中多种超痕量POPs的分析.应用灵敏度高、选择性更好的GC-MS/MS对样品中的PCBs和OCPs等进行分析,进一步降低基质的干扰.方法经过小牛血清加标实验验证,稳定可靠.POPs的加标回收率分别为88.7％～98.8％(PBDEs), 88.5％～92.5％(HBCDs), 67.9％～82.3％(PCBs)和81.7％～116.1％(OCPs),方法检出限分别为0.13～1.8 pg/mL(PBDEs), 0.31～1.2 pg/mL(HBCDs), 0.22～1.4 pg/mL(PCBs)和0.20～1.5 pg/mL(OCPs).采用本方法对潍坊地区20例母乳样品进行分析,结果显示,潍坊市母乳中HBCDs, PBDEs, PCBs、HCHs和DDTs的中值浓度分别为2.86, 7.76, 8.84、140和503 ng/g 脂重,此浓度水平与国内其它地区人群相当.     

Isolation of Lipophilic Persistent Organic Pollutants From Human Breast Milk

Background: Lipid removal from biological samples can be achieved by addition of concentrated sulfuric acid. However, certain persistent organic pollutants (POPs) such as chlorophenols are decomposed by sulfuric acid treatment and, thus, a more gentle lipid reduction method is needed for extraction of many environmental contaminants from biological samples. Membrane dialysis extraction (MDE) is a non-disruptive method to extract POPs from biological matrices.

Methods: Human breast milk samples were spiked with radiolabelled p,p′-dichlorodiphenyl trichloroethane ([C-14]-DDT) as a POP proxy and extracted using solid phase extraction (SPE). The extracts obtained were dialyzed by MDE in low-density polyethylene tubings containing a mixture of n-hexane and dichloromethane for 24 h, 48 h, or 72 h.

Results: The lipid content was reduced by 86.2% after one dialysis cycle of 24 h using MDE, and 87.1% recovery of the [C-14]-DDT standard was obtained. The DDT recovery could be further increased up to 96.3% and 98.1% by repeating the dialyses for one or two more cycles, respectively. However, the increased [C-14]-DDT recovery includes a concomitant increase in lipid carryover from 13.8% with one dialysis cycle to 22.1% with three cycles.

Conclusion: An SPE procedure for extracting POPs from breast milk and dialytic conditions for isolation of the extracted POP with minimal lipid carryover was established. The method is nondestructive and acceptable recoveries can be obtained within a single solvent shift as demonstrated by spiking standards. The lipid carryover was minimized, and the method may be considered for lipid removal before HPLC or GC analysis of environmental contaminants.     

Simple and Rapid Method for Determination of Selenium in Breast Milk by HG-AFS

A digestion procedure using H₂SO₄/HNO₃/H₂O₂ was found to be effective for destruction of human milk samples. In conjunction with a sensitive hydride generation atomic fluorescence spectrometry detection system, it is suitable for determination of selenium in those samples where the available mass of breast milk and the low selenium concentration are limiting factors. Only 1g of milk sample is needed. The procedure is simple, rapid and of low contamination potential since it is performed in the same Teflon tube from weighing to measurement. The digestion of 20 samples is completed in three hours. The detection limit is 0.25±0.04ngg^–1 of a measured solution of sample or 2.5ngg^–1 of milk. The relative uncertainty is 10% (coverage factor of 2.3, 95% probability). Because of these advantages the method is particularly suitable for epidemiological studies. The mean concentration of selenium in 62 samples of human milk from lactating women residing in the North East of Italy was 12±3ngg^–1, which is in the range of reference data.     

深圳市母乳中铅水平的调查分析

采用原子吸收法测定了深圳市300例母乳中的铅含量。结果表明,小于100μg/kg有297人,100～317μg/kg有3人;深圳市2月龄母乳喂养的婴儿在铅含量水平上是处于安全喂养水平,但是以私家车作为主要外出工具的受试者乳铅含量水平要高于其它各组,因此需要加强深圳市儿童铅含量水平的长期监测和环境铅污染治理工作。     

Application of d-SPE before SPE and HPLC-FLD to Analyze Bisphenols in Human Breast Milk Samples

In this study, we propose a simple, cost-effective, and sensitive high-performance liquid chromatography with fluorescence detection (HPLC-FLD) for the simultaneous determination of seven bisphenols (bisphenol F (BPF), bisphenol E (BPE), bisphenol B (BPB), BADGE (bisphenol A diglycidyl ether), BADGE∙2H₂O, BADGE∙H₂O, BADGE∙2HCl) in human breast milk samples. The dispersive solid phase extraction (d-SPE) coupled with solid phase extraction (SPE) procedure performed well for the majority of the analytes with recoveries in the range 57–88% and relative standard deviations (RSD%) of less than 9.4%. During the d-SPE stage, no significant matrix effect was observed thanks to the application of different pairs of salts such as zirconium-dioxide-based sorbents (Z-Sep or Z-Sep +) and primary secondary amine (PSA) or QuEChERS Enhanced Matrix Removal-Lipid (EMR-Lipid) and PSA. The method limits of quantification (mLOQs) for all investigated analytes were set at satisfactory low values in the range 171.89–235.11 ng mL⁻¹. Analyte concentrations were determined as the average value from human breast milk matrix samples. The results show that the d-SPE/SPE procedure, especially with the application of EMR-Lipid and PSA, could be used for further bisphenol analyses in human breast milk samples.     

高效液相色谱法测定胃液中甲硝唑浓度

介绍了反相高效液相色谱法测定人的胃液中甲硝唑含量的方法。服药后插管抽取胃液,试样用无水乙醇沉淀蛋白,离心,过滤,进样测定。方法的线性范围为２．５～２００ｍｇ／Ｌ,最小检知量为０．４ｍｇ／Ｌ,平均回收率为９６．０％,变异系数为３．０７％。     

人乳中蛋白质的组成分析

在对人乳样品分离与纯化的基础上,采用“Bottom Up”并结合高效液相色谱（HPLC）和配有纳米喷雾（Nano-spray）技术的高分辨傅里叶变换离子回旋共振质谱（FT-ICR-MS）,将人乳各部分蛋白质样品酶解成多肽片段。 利用碰撞活化解离（CAD）和电子捕获解离（ECD）2种解离方式断裂机理的互补性规律,借助Mascot软件数据库,快速分析了人乳样品中乳脂部分、乳清部分和乳粒部分所含主要蛋白质的组成。人乳样品各部分的共同物性是均含有多种角蛋白、乳白蛋白、乳铁蛋白,但含量和种类各有不同,这既表明了人乳特殊的营养成分,又从另一角度显示出人乳各个部分营养价值的差异。     

孕期乳房按摩对促进母乳喂养的效果研究

目的研究孕期乳房按摩对促进母乳喂养的效果。方法选取2014年3月—2014年12月在广东省清远连州市妇幼保健院定期检查并怀孕36周的产妇84例作为研究对象,抽签随机分为观察组与对照组,每组42例。对观察组每天进行乳房与乳头按摩1~2次(37周前不作乳头按摩);对照组不作乳房乳头按摩,仅采取常规的孕期检查与护理。比较两组产妇产后泌乳始动时间、始动泌乳量、纯母乳喂养率以及不同喂养方式对婴儿体内血红蛋白数、钙、锌、铁含量的影响。结果泌乳始动时间观察组(15.9±2.6)h快于对照组(24.4±2.7)h;始动泌乳量观察组(24.61±4.95)m L多于对照组(13.27±4.56)m L,两组比较均有统计学意义(P0.05)。6个月纯母乳喂养率观察组92.8%高于对照组61.9%,两组比较有统计学意义(P0.05)。6个月母乳喂养的婴儿血红蛋白数、钙、锌、铁含量均高于人工喂养的婴儿,比较有统计学意义(P0.05)。结论孕期乳房按摩对母乳喂养的促进效果显著,能明显加快泌乳始动时间,提高始动泌乳量,增加纯母乳的喂养率,提高婴儿体内血红蛋白数、钙、锌、铁含量。     

Determination of secnidazole in human plasma by high-performance liquid chromatography with UV detection and its application to the bioequivalence studies

A simple, accurate, precise and sensitive HPLC-UV method was developed for the determination of secnidazole in human plasma. Secnidazole and tinidazole (IS) were extracted from 0.2 mL of human plasma by ethyl acetate. Secnidazole was then separated by HPLC on a Diamond C(18) column and quantified by ultraviolet detection at 319 nm. The mobile phase consisted of acetonitrile-aqueous 5 mm sodium acetate (30:70, v/v) containing of 0.1% acetic acid adjusted to pH 4.0, and the flow rate was 1.0 mL/min. The low limit of quantification was 0.1 microg/mL. The method was linear over the concentration range 0.1-25.0 microg/mL (R(2) = 1.000). The recovery of secnidazole from human plasma ranged from 76.5 to 89.1%. Inter- and intra-assay precision ranged from 3.3 to 10.7%. Secnidazole in plasma was stable when stored at ambient temperature for 8 h, at -20 degrees C for 2 weeks and at -20 degrees C for three freeze-thaw cycles. The developed method was successfully applied to the pharmacokinetic and bioequivalence studies between test and reference secnidazole tablets following a single 500 mg oral dosage to 20 healthy volunteers of both genders. Pharmacokinetics parameters T(max), C(max), AUC(0-)t, AUC(0-infinity), T(1/2) were determined of both preparations. The analysis of variance (ANOVA) did not show any significant difference between the two preparations and 90% confidence intervals fell within the acceptable range for bioequivalence. It was concluded that the two secnidazole preparations are bioequivalence and may be used interchangeably.