尿中氯胺酮及其代谢物盘鉴和GC/MS/SIM测定

目的 研究尿中氯胺酮(KET)及其代谢物去甲基氯胺酮(NKET)的盘鉴(Disk SPE)。方法 用含有化学键合C18和强酸型强阳离子交换(SCX)基团的萃取柱SPEC.C18 AR/MP3萃取,加入萃取柱前的尿样用0.1mol/L磷酸盐缓冲溶液(pH 6)稀释,洗脱溶剂为含2％(v/v)氨水的乙酸乙酯;以2,4,6-三硝基甲苯(TNT)为色谱内标,GC/MS/SIM检测。结果 在加标量为0.5μg/mL、2μg/mL和6μg/mL的控制尿样中,KET和NKET的平均回收率分别为91.5％和79.9％,6次测定的RSD均为8.7％;线性范围0.02-8μg/mL,线性相关系数分别为0.9819和0.9964;检出限(S/N=3)分别为6ng/mL和4ng/mL;总离子色谱图背景低,杂质少。同一根萃取柱重复使用8次以上未见性能下降;嫌疑尿样中检出KET和/或NKET,和常规的液液萃取结果相符。结论 该方法适用于尿中KET和NKET的同时测定。     

Phenibut screening and quantification with liquid chromatography–tandem mass spectrometry and its application to driving cases

An analytical strategy for identification by an LC–MS/MS multitarget screening method and a suitable LC–MS/MS based quantification were developed for the psychotropic drug phenibut. The samples analyzed were collected during traffic control and were associated with driving under the influence of drugs. A positive sample for phenibut was identified in a single case of driving under the influence. The quantification revealed a drug concentration of 1.9 μg/mL. An interaction with blood alcohol (BAC = 0.10%) was discussed as the explanation of the way of driving and deficit manifestations observed (swaying, nystagmus, quivering of the eyelid, and reddened eyes). According to the available information, the quantified phenibut concentration could be explained by an intake of four tablets (self-reported) during the day containing 250 mg of the drug. Chromatography was performed with a Luna 5 μm C18 (2) 100 A, 150 mm × 2 mm analytical column, and a buffer system consisted of 10 mM ammonium acetate and 0.1% acetic acid (v/v) included in mobile phases marked as A (H₂O/methanol = 95/5, v/v) and B (H₂O/methanol = 3/97, v/v). An effective limit of detection (LOD = 0.002 μg/mL) could be achieved for the multitarget screening method. The quantification of phenibut was performed on a second LC–MS/MS system with LOD/LOQ values of 0.22/0.40 μg/mL. Since phenibut quantification data are rare, the presented information can be used with caution for evaluation of positive cases in the future.     

Variability of simulants used in recreating stab events

Formic acid (FA) concentration was measured in post-mortem blood and urine samples as methyl formate using a headspace in-tube extraction gas-chromatography-mass-spectrometry method. A total of 113 cases were analyzed, each including a blood and urine sample fortified with 1% sodium fluoride. The cases were divided into three groups: regular (n=59), putrefied (n=30), and methanol-positive (n=22) cases. There was no evidence of ante-mortem methanol consumption in the regular and putrefied cases. In regular cases, the mean (and median) FA concentrations were 0.04 g/l (0.04 g/l) and 0.06 g/l (0.04 g/l) in blood and urine, respectively. In putrefied cases, the mean (and median) FA concentrations were substantially higher, 0.24 g/l (0.22 g/l) and 0.25 g/l (0.15 g/l) in blood and urine, respectively. In three putrefied cases, FA concentration in blood exceeded 0.5 g/l, a level associated with fatal methanol poisoning. Ten putrefied cases were reanalyzed after 3-4 months storage, and no significant changes in FA concentrations were seen. These observations suggest that FA was formed by putrefaction during the post-mortem period, not during sample storage when sodium fluoride was added as a preservative. In methanol-positive cases, the mean (and median) FA concentrations were 0.80 g/l (0.88 g/l) and 3.4 g/l (3.3 g/l) in blood and urine, respectively, and the concentrations ranged from 0.19 to 1.0 g/l in blood and from 1.7 to 5.6 g/l in urine. The mean (and median) methanol concentrations in methanol-positive cases were 3.0 g/l (3.0 g/l) and 4.4 g/l (4.7 g/l) in blood and in urine, respectively. The highest methanol concentrations were 6.0 g/l and 8.7 g/l in blood and urine, respectively. No ethyl alcohol was found in the methanol-positive blood samples. Poor correlation was shown between blood and urine concentrations of FA. Poor correlations were also shown, in both blood and urine, between methanol and FA concentrations.     

SPE—GC／MS、GC／NPD法检测血液中苯丙胺类毒品

目的利用GC／MS、GC／NPD与固相萃取（SPE）技术相结合,建立血液中苯丙胺类毒品的定性定量分析方法。方法采用Bond—ElutCerti{y固相柱、甲醇淋洗、二氯甲烷／异丙醇／氨水（78／20／2）洗脱固相萃取分离提取,比较了不同PH体系、稀释状态、洗脱溶剂对提取回收率的影响,建立血液中苯丙胺类毒品的GC／MS、GC／NPD定性定量分析方法。结果以GC／NPD分析AM、MA、MDA和MDMA浓度在15ng／mL-2000ng／mL、10ng／mL～1600ng／mL、20ng／mL-3000ng／ml、20ng／mL-3000ng／mL范围内线性关系良好,AM、MA、MDA和MDMA的检测限分别为10ng／mL、8ng／mL、15ng／mL、15ng／mL,方法平均回收率大于85％,标准偏差小于5％,GC／MS-Scan检测限分别为40ng／mL、32．0ng／mL、60．0ng／mL、60．0ng／mL。结论此方法可满足苯丙胺类毒品滥用者的血液定性定量分析。     

HS-SPME-GC/MS联用法测定生物检材中的百草枯

目的建立检测生物检材中百草枯的顶空固相微萃取-气相色谱-质谱联用（HS-SPME-GC/MS）的分析方法。方法尿样中加乙基百草枯作为内标,在氯化镍作催化剂的条件下,用硼氢化钠在碱性条件下进行还原,HS-SPME萃取,提取物经GC/MS分析。全血需先离心,沉淀血细胞提取上清液,再用甲醇沉淀蛋白。最终得到的上清液加内标乙基百草枯,以下操作同尿样。结果尿样和血样中的百草枯的还原产物在1.0μg/mL~100μg/mL范围内线性关系良好,回归方程分别为y=0.0957x-0.0163,r=0.9974（n=6）;y=0.1096x＋0.0871,r=0.9964（n=6）。尿样、血样低、中、高三个质量浓度,RSD值均小于7%。回收率分别为尿样85.49%~100.83%,血样94.72%~99.68%。结论本法操作简便易行、灵敏度高、快速准确。为检测生物检材中的百草枯提供了有效的方法。     

反相高效液相色谱法测定人血浆中的吲哚美辛

建立血浆中吲哚美辛的高效液相色谱分析方法 ,扩大药 (毒 )物检测范围及手段 ,以适应法医学鉴定的特殊需要。以空白血浆标准添加吲哚美辛对样品处理方法、线性关系、回收率及精度进行考察 ,并以所建方法对健康受试者的血液浓度进行监测。方法的线性范围是 0 1～ 5 0 μg·ml-1,γ =0 9995 ,最小检出浓度为 0 0 2 μg·ml-1(S/N≥ 3)。日内、日间的方法精密度为 ( 1 1± 0 2 ) % (n =4)和 ( 2 7± 0 6 ) % (n =4) ,加样回收率为 97 5 %～10 4 2 %。所建方法准确、便捷、选择性好 ,可用于法医学鉴定及血液浓度监测     

GC/MS法检测全血中的奥氮平

目的采用乙睛-甲醇混合溶剂提取、气质联用分析法检测全血中奥氮平。方法针对奥氮平特性,在加入稳定剂硫代硫酸钠条件下采用乙睛-甲醇混合溶剂提取法,采用GC/MS分析法,对全血中的奥氮平进行定性、定量分析。并对提取介质、酸碱度、稳定剂种类及用量进行了考察。结果采用本文方法在奥氮平为1～400μg/mL浓度范围内呈良好的线性关系(r2=0.999 8,n=5),检出限为1.0ng,方法平均回收率可达66.5%(RSD=2.5%)。日内RSD为2.1%～3.9%,日间RSD为2.9%～4.5%。选择乙腈∶甲醇(V∶V=8∶2)混合溶剂进行液-液提取,稳定剂为300mg硫代硫酸钠。结论本文方法可用于全血中奥氮平检测,在相关案件检验中选择使用。     

气相色谱法同时测定血清中甲醇、乙醇、正丙醇

目的建立气相色谱同时测定血清中甲醇、乙醇、正丙醇含量的方法。方法改变气相色谱条件,以异戊醇为内标,采用气相色谱一氢火焰离子化检测器对血清直接进行检测。并通过待测组分与内标物的响应值比进行定量。结果GC／FID法检测血清中的甲醇、乙醇、正丙醇含量,得到了良好的线性关系。乙醇浓度从1～100mg／100ml。的线性关系式为Y=0．4145X＋0．0232（R2=0．9974）、浓度从100～1000mg／100mL的线性关系式为Y=0．4511X＋0．0746（R2=0．9911）,甲醇浓度从l-200mg／100mL的线性关系式为Y=0．2778X＋0．0493（R2=0．9983）。结论该方法操作简便快速,重现性好,通过检测正丙醇还可以推断腐败血样自身产生的乙醇量,是一种较为理想的血醇检测方法。     

生物检材中乌头碱的LC-MS/MS快速分析

目的应用高效液相色谱-质谱法对生物检材中乌头生物碱等有毒成分进行快速分析。方法取全血样品经乙腈-甲醇(5:1 v/v)提取,使用Agilent Zorbax SB C18(2.1 mm×50 mm,1.8μm)色谱柱,以0.1%甲酸溶液-乙腈(60:40 v/v)为流动相等度洗脱。在多反应监测模式下测定全血样品中乌头生物碱等有毒成分。结果乌头碱、次乌头碱和中乌头碱的保留时间为0.73 min、0.77 min和0.63 min;用于定量分析的离子对分别为m/z 646.4→586.4(乌头碱)、616.1→556.5(次乌头碱)和632.4→572.1(中乌头碱)。乌头碱在0.1~250 ng/m L内线性关系良好,相关系数(r)≥0.9987,最低检出限0.1ng/m L,精密度考查其变异系数(CV)5.42%(n=6),血液中乌头碱提取回收率不小于90%。结论本文建立的高效液相色谱-质谱法快速、简便、灵敏,适用于天然药毒物检验。     

分子印迹固相萃取法在血中苯丙胺类毒品分析中的应用

目的建立分子印迹固相萃取（MISPE）、GC/MS分析方法,用于血液中苯丙胺类毒品检测。方法 10mmol/L醋酸铵缓冲液（pH8.0）4倍稀释空白添加血液,1mL甲醇,1mL10mmol/L醋酸铵缓冲液（pH8.0）活化苯丙胺类分子印迹固相萃取柱;2×1mL去离子水、1mL60%的乙腈去离子水、1mL1%醋酸乙腈洗涤杂质;2×1mL1%甲酸/甲醇洗脱,洗脱液挥干定容,经GC/NPD、GC/MS分析检测。结果各种苯丙胺类毒品回收率均在90%以上,在20～5 000ng/mL浓度范围内线性关系良好,r2为0.995 7～0.998 9,LOQ在16～30ng/mL之间,LOD在8～15ng/mL之间。结论本方法回收率高,净化效果显著,稳定性好,杂质干扰少,可用于血液中低浓度苯丙胺类毒品的分析检测。     

全血中利多卡因的高效液相色谱法测定

本文报道反相高效液相色谱法测定全血中利多卡因浓度的方法。氟安定作为内标,全血经溶血,1N 氢氧化钠1ml 碱化后,用乙醚提取。以Zorbax ODS 为固定相,以CH_3 OH∶H_2O∶(C_2H_5) _3N(100∶45∶0. 2,pH6. 3) 为流动相,检测波长为240nm。用利多卡因为内标的峰高比定量。血中利多卡因最低检出浓度为0. 125ug/ml。线性范围是0. 0025～0. 0750mg/ml(r=0. 9999) 和0. 0250～0. 3000mg/ml(r=0. 9999) 。本法添加利多卡因1. 0、2. 5,8. 0ug 的回收率分别为101. 51±1. 51%、98. 10±2. 05%和±98. 09±3. 63%,天内变异系数分别为1. 49、1. 29和3. 70,天间变异系数为1. 78%。     

The relationship of methanol and formate concentrations in fatalities where methanol is detected

An automated headspace gas chromatography method was developed for the determination of formate (formic acid) in postmortem specimens, based on the in situ sulfuric acid-methanol methylation of formic acid to methyl formate. Diisopropyl ether was used as an internal standard. The method was applied to over 150 postmortem cases where methanol was detected. Of the 153 cases presented, 107 deaths were attributed to acute methanol toxicity. In the vast majority of the remaining 46 deaths, the methanol was determined to be present as a postmortem or perimortem artifact, or was otherwise incidental to the cause of death. Of the 76 victims who were found dead and blood was collected by the medical examiner, all but one had a postmortem blood formate concentration greater than 0.50 g/L (mean 0.85 g/L; n = 74). The sole exception involved suicidal ingestion of methanol where the blood methanol concentration was 7.9 g/L (790 mg/100 mL) and blood formate 0.12 g/L. In 97% (72/74) of the cases where blood was available, the blood formate was between 0.60 and 1.40 g/L. In 31 of the 153 cases, the victim was hospitalized and blood obtained on admission or soon after was analyzed for methanol and formate during the subsequent death investigation; the vast majority (27/30) had antemortem blood formate concentrations greater than 0.50 g/L. Cases with samples taken prior to death with blood formate concentrations less than 0.5 g/L can readily be explained by active treatment such as dialysis. The blood formate method has also been useful in confirming probable perimortem or postmortem contamination of one of more fluids or tissues with methanol (e.g., windshield washer fluid or embalming fluid), where methanol ingestion was unlikely.     

Determination and validation of tetrodotoxin in human whole blood using hydrophilic interaction liquid chromatography-tandem mass spectroscopy and its application

A sensitive analytical method was developed for the quantitative determination of tetrodotoxin (TTX), a powerful sodium channel blocker, in human postmortem whole blood. The sample mixture was cleaned up using cation exchange SPE catridge after protein precipitation by methanol and then separated on a PC-HILIC (phosphorylcholine hydrophilic interaction liquid chromatography) column (150 mm × 2.0mm i.d., 5 μm) using a isocratic elution of 1% acetic acid and acetonitrile. The identification of TTX was performed on tandem mass spectrometry with electrospray ionization interface in positive ion mode. The retention time of voglibose (internal standard) and TTX was 5.1 and 6.0 min, respectively. TTX and internal standard (voglibose) were monitored and quantitated using the ion transitions: the respective precursor to product ion combinations, m/z 320/302 for TTX and m/z 268/92 for voglibose in the multiple reaction monitoring (MRM) mode. The recovery of TTX and voglibose was 61.4% and 62.8%, respectively and the good accuracy (97.7-103.9%), linearity (2-1200 ng/mL) and reproducibility were shown in this method. The limit of detection and limit of quantification were 0.32 ng/mL and 1.08 ng/mL, respectively. This method was applied in the case of three fishermen who were poisoned (including one death) by unknown fish on their boat in October 2010. In this case, the levels of TTX were 27.2, 30.0 and 29.7 ng/mL in heart blood, peripheral blood and serum of a victim, were 3.1 and 12.1 ng/mL in peripheral blood and 3.9 and 12.8 ng/mL in serum of two survivors, respectively.     

Aqueous phase hexylchloroformate derivatization and solid phase microextraction: determination of benzoylecgonine in urine by gas chromatography-quadrupole ion trap mass spectrometry.

A derivatization/solid phase microextraction (SPME) method for the determination of benzoylecgonine in urine was developed. The derivatization is conducted directly in 1 mL of urine while sonicating for 3 min with 12 microL of hexyl chloroformate and 70 microL of a mixture containing acetonitrile:water:hexanol:2-dimethylaminopyridine (5:2:2:1 v/v), yielding benzoylecgonine hexyl ester (BHE) as the product. After the 3 min period, an aliquot of 250 microL is transferred to a vial for SPME. After the desired extraction time the 100 microns polydimethylsiloxane SPME fiber was transferred to the GC-MS for separation and analysis with a quadrupole ion trap mass spectrometer. The hexyl chloroformate derivatization and SPME procedures were optimized for compatibility and sensitivity. The method was found linear for 0.10 to 20.0 micrograms/mL (r2 = 0.999) of benzoylecgonine in urine using benzoylecgonine-d3 as an internal standard (1.5 micrograms/mL). Intra-day precisions were 8.8 and 6.8% RSD for 0.30 microgram/mL and 17 micrograms/mL benzoylecgonine standards in urine (n = 6), respectively. Inter-day precision (n = 3) were < or = 3.3% RSD, indicating good reproducibility. A detection limit of 0.03 microgram/mL (S/N = 3) was achieved, thus making the SPME method a simplified alternative to SPE for GC-MS confirmation after EMIT tests for benzoylecgonine which have a cutoff of 0.30 microgram/mL. Quantitative results by SPME and SPE of two clinical urine specimens known positive for cocaine by EMIT were in excellent agreement. Benzoylecgonine was detected by the derivatization/SPME method in 22 out of 22 other urine specimens known positive for cocaine.     

UPLC-MS/MS法检测血痕中常见烟草、毒品和药物成分

目的建立UPLC-MS/MS测定血痕中尼古丁、可替宁、甲基苯丙胺、氯胺酮、吗啡、O6-单乙酰吗啡、地西泮、三唑仑、艾司唑仑、佐匹克隆和利血平的方法。方法以甲醇为提取液,采用基质提取溶液配制标准溶液制作定量曲线。采用超高效液相色谱柱对待测样品进行分离;以电喷雾离子源正离子（ESI＋）模式和多反应监测（MRM）模式进行质谱分析。优化实验条件,并进行方法学评价。结果选择UPLC HSS T3色谱柱,乙腈-5mmol/L甲酸铵＋0.1%（v/v）甲酸作为流动相,甲醇作为提取溶剂。11种检测物检出限（S/N=3）和定量限（S/N=10）分别为0.04~2.82ng和0.13~7.64ng,1~500ng/mL范围内的线性关系良好。除利血平、吗啡外的检测物回收率为（53.8±5.3）%~（107.2±12.6）%。结论采用本文UPLC-MS/MS方法对血痕中11种常见烟草、毒品和药物成分进行检测,能够满足实际检案的要求,可在相关检验中选用。     

腐败生物检材中多种碱性滥用药物的检测

目的建立腐败生物检材中多种碱性滥用药物的提取、净化和仪器分析方法。方法用环己烷作为提取溶剂液-液萃取,同时采用Bond Elut Certify小柱、甲醇淋洗、二氯甲烷：异丙醇：氨水（78：20：2）洗脱固相萃取分离提取,GC／MS、GC／NPD定性定量分析各种生物检材中的滥用药物。结果从所送死者肝组织、胃组织、心血及胃内容、尿样、各检材中均同时检出吗啡、可待因、舒乐安定和异丙嗪成份,其中肝组织含量分别为吗啡0．094μg／g、可待因0．257μg／g、异丙嗪0．110μg／g,尿液含量分别为吗啡0．334μg／ml、可待N4．054μg／ml、异丙嗪0．066μg／ml,心血含量分别为吗啡0．036μg／ml、可待N0．106μg／g、异丙嗪0．088μg／ml。结论此方法准确、可靠、科学,可以用于法医毒物分析领域体内检材多种碱性药物的检测。     

Examination of the effect of dose-death interval on detection of meperidine exposure in decomposed skeletal tissues using microwave-assisted extraction

The effect of dose-death interval and tissue distribution on the detection of meperidine in selected skeletal tissues was examined using a rapid microwave-assisted extraction (MAE) methodology. Rats (n=14) were dosed with 0 (n=2) or 30 mg/kg (n=12) meperidine (i.p.). Drug-positive rats were sacrificed with CO(2) after 20, 30, 90 and 150 min (n=3 per group). Heart blood was collected immediately after death. Tibiae were excised and frozen for further analysis. The remaining carcasses were allowed to decompose outside in secured cages to the point of complete skeletonization in a rural Northern Ontario location during the late summer months. Vertebrae and pelvi were collected for each animal. Tibial marrow was homogenized in 3 mL PB6 (phosphate buffer, 0.1M, pH 6). Fresh tibiae, and decomposed vertebrae and pelvi were cleaned in PB8.5 (phosphate buffer, 0.1M, pH 8.5) and sonicated to remove remaining soft tissue. Samples of dried, ground bone (0.5-1g) suspended in 2 mL PB6 were then irradiated in a domestic microwave oven (1100 W) at atmospheric pressure for 15 min. Samples of vertebral bone (1g) were also extracted by passive incubation in methanol (3 mL, 50°C, 72 h). All supernatants then underwent solid-phase extraction and analysis by GC/MS, using electron impact ionization in the Selected Ion Monitoring (SIM) mode. Mean GC/MS responses for each tissue type were negatively correlated with dose-death interval, with correlation coefficients ranging from -0.32 to -0.87. Analysis of variance showed dose-death interval to be a main effect (p<0.05) with respect to GC/MS response for blood, marrow, tibial epiphyses prepared by MAE, and vertebral bone prepared by passive extraction, but not for tibial diaphyses, pelvi or vertebrae prepared by MAE. Overall, MAE is advantageous as a rapid extraction tool for screening purposes in skeletal tissues, but assignment of significance to quantitative expressions of skeletal drug concentrations is complex and should be approached with caution.     

Solid-phase extraction and analysis of 20 antidepressant drugs in human plasma by LC/MS with SSI method

A simultaneous determination of 20 antidepressant drugs (imipramine, amitriptyline, desipramine, trimipramine, nortriptyline, clomipramine, amoxapine, lofepramine, dosulepin, maprotiline, mianserin, setiptiline, trazodone, fluvoxamine, paroxetine, milnacipran, sulpiride, tandspirone, methylphenidate and melitracen) in human plasma was developed using LC/MS with sonic spray ionization (SSI) method. These drugs showed good separation and sensitivity by LC-MS using an Inertsil C-8 column with methanol:10mM ammonium acetate (pH 5.0):acetonitrile (70:20:10) as mobile phase at 0.10 mL/min at 35 degrees C. Solid-phase extraction of these drugs added to the human plasma was performed with an Oasis HLB cartridge column. Recovery and limit of detection of these drugs were between 69 and 102% and between 0.03 and 0.63 microg/mL, respectively. The present procedure offers an easier and more convenient screening method for antidepressants, and will be useful for forensic toxicology investigations.     

Potential for error when assessing blood cyanide concentrations in fire victims.

The present study explores toxicologic significance of blood cyanide concentrations in fire victims. Headspace gas chromatography was used for cyanide detection. Analysis of blood samples from ten fire victims (postmortem interval = 8 h to 3 to 5 d) detected zero to 11.9 mg/L of cyanide and a large difference in cyanide concentrations among victims. Carboxyhemoglobin (COHb) saturation was in the range of 24.9 to 84.2%. To examine the effects of methemoglobinemia and postmortem interval on blood cyanide concentrations in fire victims, an experiment was carried out using rabbits as the animal model. The rabbits were sacrificed by intramuscular injection of 1 mL/kg 2% potassium cyanide 5 min after intravenous injection of 0.33 mL/kg of 3% sodium nitrite (Group A, n = 3) or physiological saline (Group B, n = 6). Average methemoglobin contents immediately before potassium cyanide administration were 6.9 and 0.8% in Groups A and B, respectively. Average cyanide concentrations in cardiac blood at the time of death were 47.4 and 3.56 mg/L, respectively. When blood-containing hearts of the rabbits (n = 3 for Group B) were left at 46 degrees C for the first 1 h, at 20 to 25 degrees C for the next 23 h and then at 4 degrees C for 48 h, approximately 85 and 46% of the original amounts of blood cyanide disappeared within 24 h in Groups A and B, respectively. After the 72-h storage period, 37 and 10%, respectively, of the original amounts of cyanide remained in the blood. When the other three hearts in Group B were left at 20 to 25 degrees C for the last 48 h without refrigeration, cyanide had disappeared almost completely by the end of the experiment. The present results and those published in the literature demonstrate that the toxic effects of cyanide on fire victims should not be evaluated based solely on the concentration in blood.     

UFLC法测定新型“spike99”香料中JWH-073的含量

目的 超快速液相色谱法测定新型“spike99”香料中JWH-073的含量.方法 采用Shim-pack XR-ODSⅡ色谱柱(2.0mm×75mm,2.2μm);流动相:乙腈(含0.1％甲酸):水(含0.1％甲酸)(80∶20,v/v),流速:0.25 mL/min;检测波长280nm,柱温:35℃,进样量:2μL,外标法定量测定JWH-073的含量.考查方法的线性范围、灵敏度、精密度、回收率和稳定性,并用于检测实际案例样品.结果 JWH-073浓度在1～50μg/mL范围内线性良好(A=9 398.7C-635.75,r =0.999 9);最低检测限为100ng/mL(S/N=3);低、中、高3种浓度的加样回收率(n=3)分别为100.52％(RSD=0.36％),99.52％(RSD =0.43％),99.03％(RSD =0.17％).结论 本法测定新型“spike99”香料中JWH-073含量操作简便、灵敏、准确,重复性好,适于在相关案件检验中选用.