ashes of sojourn

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Ruth J. H. Waddell-Smith, Ph.D. A Review of Recent Advances in Impurity Profiling of Illicit MDMA Samples ABSTRACT: Profiling illicit ecstasy tablets has the potential to become an invaluable tool in the crackdown on drug trafficking, but that potential has yet to be fully realized. The impurity profile of an ecstasy tablet can be used to determine the method employed to synthesize the actual con- trolled substance, which in most cases, is 3,4-methylenedioxymethamphetamine (MDMA). Tablets can then be linked to a common synthetic route, potentially to a common manufacturer, and possibly even to a common manufacturing batch, based on the impurities present. Current methods for profiling MDMA tablets typically involve extracting the organic impurities for analysis by gas chromatography-mass spectrometry. The potential of profiling the trace metals present in tablets has begun to be investigated while more robust statistical and chemometric procedures are being applied to compare and link tablets. This article reviews the recent advances in MDMA impurity profiling from 2002 up to the end of 2006. KEYWORDS: forensic science, MDMA, organic impurity profiling, trace metal impurity profiling, chemometric procedures Initially synthesized by Merck (Whitehouse Station, NJ) in an attempt to develop new synthetic routes for blood clotting agents, 3,4-methylenedioxymethamphetamine (MDMA) has never actually been marketed (1). Today, MDMA has no legitimate medical use and is probably best known as the controlled substance in the club drug ‘‘ecstasy.’’ A report published by the United Nations Office on Drugs and Crime indicated that regional differences in tablet composition were apparent: in East South South-East Asia, the term ‘‘ecstasy’’ is used to refer to any drug tablet, irrespective of the presence of MDMA, while in Europe and North America, there is a trend toward high purity ecstasy tablets containing only MDMA (2). Several authors have also reported trends in the com- position of ecstasy tablets, in Europe, Asia, and North America (3–7). In almost all cases, MDMA was reported as the principal active ingredient, although other controlled substances may be pres- ent, for example 3,4-methylenedioxymethamphetamine (MDA), methamphetamine, ketamine, or amphetamine (7,8). According to the 2005 midyear report published by the National Forensic Laboratory Information System, the number of MDMA exhibits seized in the United States decreased significantly between 2001 and the second quarter of 2005 (9). However, through Janu- ary to June 2005, MDMA was the most commonly encountered club drug across all regions of the United States, constituting 88% of club drugs in the West, 86% in the South, 84% in the Midwest, and 64% in the Northeast (9). With this in mind, the need to crack- down on manufacturers to eliminate production and trafficking, both at the local and national levels, is apparent. In the past, profiling of illicit tablets to identify a common source was based on a physical description of the tablet (10). How- ever, physical characterization is limited as tablets with the same physical characteristics, such as dimension, mass, color, and motif, do not necessarily have the same chemical composition (3). Hence, profiling has moved toward chemical characterization of tablets, based on the impurities and by-products present as a result of the synthetic method (e.g., (3,11–14)). Likely sources of organic impurities include products from side reactions, poor chemical han- dling during synthesis, inadequate purification procedures, and con- tamination, which may be from contaminated reactants and materials, as well as effects from packaging, handling, and storage. Some impurities are specific to a particular synthetic route and are used as markers for profiling purposes. Tablets containing con- trolled substance produced in the same manufacturing batch are expected to contain similar levels of the same impurities and hence will have similar impurity profiles (13). Batches produced using different synthetic methods and or in different laboratories are expected to yield significantly different impurity profiles (13). Organic impurity profiling of illicit ecstasy tablets in this way has proven successful in differentiating routes used to synthesize the MDMA, in both laboratory synthesized and seized samples (12,13,15,16). More recently, the potential of identifying links among illicit drug seizures based on trace metal impurities has been investigated (17–26). While the initial potential of this method has been demon- strated, more thorough research is required to fully develop its potential. With optimization and validation of appropriate method- ologies, routine trace metal profiling of illicit MDMA tablets is not out of reach. A recent paper reviewed the analytical and chemometric meth- ods used to profile illicit drug seizures up to and including 2002 (27). This paper does not intend to repeat the previously reported literature; rather, it is intended to make the reader aware of the most current research in this field, while also making recommenda- tions as to the future direction for MDMA profiling. Organic Impurity Profiling Organic impurity profiling has mainly been based on liquid– liquid extractions of the impurities, followed by gas chromatogra- phy-mass spectrometry (GC-MS) analysis. While early profiling attempts identified potential synthetic route markers, todays researchers are going further, identifying precursors, intermediates, by-products, and excipients, thereby generating a ‘‘chemical finger- print’’ of the sample (3,11,13–16,28–30). Different synthetic routes and variations of the same route have been studied, aiming to School of Criminal Justice & Department of Chemistry, Michigan State University, 560 Baker Hall, East Lansing, MI 48824. Received 7 Jan. 2007; and in revised form 29 April 2007; accepted 29 April 2007; published 21 Dec. 2007. J Forensic Sci, November 2007, Vol. 52, No. 6 doi: 10.1111/j.1556-4029.2007.00559.x Available online at: www.blackwell-synergy.com Ó 2007 American Academy of Forensic Sciences 1297

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The world ended with fire and ash. Now, only the ash remains. The tale of a vagrant and his follower.

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Page 1: Ashes of Sojourn

SojournEpisode One: RaindropsIt was raining that day... Not the life-giving rain I'd enjoyed inmy youth... No, this rain was white as snow with the bitter taste of ash, tainted by the death that had claimed everything.My cloak was soaked, with a layer of ashen grime upon it. Mypack, heavy to begin with, was now heavier with the added weight of the water in it. I'd given up on finding shelter long before then, so I no longer hastened my footsteps. At least the rain was a summer one, I told myself bitterly.I'd noticed the scent of rain earlier that day. Knowing this, I had still set out from the cave I'd spent the night in. A choiceI was now paying for.A sound, faint as it was, snapped me away from my thoughts. I paused, straining my ears against the soft pattering of the raindrops. Perhaps, I thought, though it was more hope than belief, I'd heard wrong...I hadn't. The sound came again, a low, deep howl, and it wascloser this time. I drew my sword slowly, watching my surroundings.Silence.Then, a rustling in the bush behind me, followed by another howl. I saw a shape emerging from the white tinted, green leaves and I swung. Only too late did I realize what the shape was.A young woman...She screamed as she saw me. It was too late for my swing tostop. Even if I tried, she was still moving too fast too avoid it.Time seemed impossibly slow, and all I could do was watch.Somehow, she slipped on the ash-colored ground, sliding right under my blade. Before I could sigh in relief, though, I saw why she'd been running. A black-haired Warg at least twice the size of any normal wolf I'd ever seen was in mid-leap behind her. Using my momentum, I continued the swingof my sword into a thrust, right into the beast's heart. I sidestepped, allowing the Warg's jump to carry its body off my sword.My attention returned to the woman, "What the hell?!" I

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demanded, "Why would you charge at someone like that?"She met the remark with eyes of fire, "What?! You nearly hit me!" She stood, shakily, "I'm fine, by the way."My stomach tightened, but I did not wish to be at a disadvantage. "Like the hell I care." I said, turning."Where are you going?" She asked."Out of this damn rain." I retorted. I was suddenly very tired.She followed me... God only knows why, but she did... And she hasn't quit...~Fin~

Episode Two: Silver LiningI sat at the mouth of the cave, watching the eternal gray of the sky.The woman was inside, drying her clothes by the fire. I'd loaned her a spare set from my pack, not wanting the situation to be any more awkward than it already was."You can look now." She said. I continued staring at the sky.The rain was falling lighter now. The sound of it wasn't as oppressive as it was before."The sky doesn't ever change, you know," She said as she sat beside me. She looked at me as if expecting an answer.I said nothing.After a while, she sighed and looked out upon the forest. For a while, all was silent."I am Erica," She stated, breaking the fragile glass that had filled the air."Call me Ross." I replied simply, trying to indicate I wished the return of silence.She gave me an odd look, what more did she wish?"No last name?""Well, Erica No-Name," I said, looking at her. "You didn't give me one. So, Ross it shall remain." I returned my gaze to the sky."What are you looking for?" She asked, following my eyes.The ash clouds shifted. My heart skipped a beat."Sometimes, after it rains," I said slowly, "You can see the sky..."

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The clouds thinned in a patch. Then, I saw it. It was there for a few seconds, and then it was gone. A small priceless treasure slipping away like sand.It was nothing more than a flash of blue and a short-lived rayof sunlight. Things that at one point had seemed mundane.Perhaps in times that are anything but ordinary, we desperately cling to things that are 'normal' because we seek an anchor... Something to tell us that the world we onceknew is still there, somewhere out there.A futile effort...~Fin~

Episode Three: NaturesThe deer nibbled at the few stalks of grass that poked through the white-gray layer of wet ash. Every few seconds it would lift its head.From my place of hiding within a stunted bush I nocked and arrow on my hunting bow. I drew it back as silently as I could, hoping the deer would not hear the creak of the wood.The shot struck with enough force to knock the animal over. Iran across the distance between us, drawing my knife. With practiced aim I ended the doe's pain.She wasn't large, but she weighed enough that I had to stop and rest once or twice before I reached the camp.The woman, Erica, was waiting for me."You save my life and now I'm your servant?" She demanded, "Why should I do laundry?"I set the deer down, rather ungently. "Because you're following me, and I have no earthly clue why. Because I shared my supplies with you." I removed a cord of rope made of vines from my bag and started fashioning a rack to smoke the meat.She grumbled, but headed off towards the stream. I smiled as a thought came to me, "Oh yeah, and because you're a woman." I called.My smile widened as I started cutting the deer.Once the meat had started the slow process of smoking and the skin tanning in the pale sunlight, I sat against a tree and

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closed my eyes. Sleep came fast.I was awakened by Erica. Not by her footsteps, no, the woman crept up to me and emptied a bucket full of ash-laden water on me. I sputtered as I snapped awake."What the hell?!"She smiled as she handed me the portable wash board, still dripping with water. "You're going to want this." She said.I ignored the board, "Where did you get the bucket?" I asked."It was half-buried by the stream.""Well, that's a good find, it holds water, keep it. Perhaps we can trade it for something." I said as I stood."With who?" She seemed puzzled."Why," I said surprised, "With other survivors, of course!" Had she thought I was the only one?~Fin~

Episode Four: Stand AloneThe day was warm, even though it held a closer resemblanceto early winter than it did the middle of summer. The ash fall of the previous night had been heavier than usual, perhaps indicating a good amount of dew.No matter what the reason, the result was the same, ankle high ash everywhere you looked. Even after years of the stuff, I hated it no less than I did the first days it had fallen. "Don't mind the ash," Someone had once told me, "You get used to it eventually." Odd as it sounded, it was true. Ash was a part of this world now, part of the life, part of me... I had grown used to it, but that didn't mean I had to like it.I must have been smiling, for Erica gave me a puzzled look, "Something funny?" She asked."Nothing." I said. The time passed by with only the sound of footsteps and birdsong to fill the empty space. Sometimes, not even that.That was how most days went. Each time, I was reminded once again that I was no longer alone in my endless wandering...And my companion seemed so unlikely... Innocent. That is the best word to describe her, I think. She was innocent to

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the ways of the world. After all that had happened, I did not find it likely that one such as she could exist, yet...One night, I found myself pondering on the way she had acted the other day when I had mentioned trading. Her reaction at the indication of other people was... Startling.Where was she from that she thought she was the only one left?Erica had a knack for detecting even the slightest changes inpeople. A talent that was more annoying than she was by itself."Ross, do you think I'm beautiful?" She asked. When I could offer no answer at first, she started giggling, "You've been staring at me, and not the way most men do... What's on your mind?"The forest had grown quiet, as if it too wished to know what was in my thoughts."I am considering where I will go next." I said, "Once we stop in Traviel, I think I'll head north, maybe to Ne'Yudan." A lie, I almost never considered where to head, but she did not know that."'I'?" She quoted, sounding hurt. "What about me?" She looked at the ground."You tell me. I don't decide your path. Hell," I shook the ash off my bedroll, "I don't even know why you're following me. From what I can tell, you seem to think you were the only person left, so I'd guess you want to stay with your kind.""My kind?" There was a slight hint of fury to her voice. "Are you not human or something?"I wanted to shake my head. Even if I explained it to her, she would never understand. "The people in the villages are..." I paused to try to organize my thoughts, "Well... They need to stay in one place. Especially after the... 'Incident'.. I am a wanderer, I can't stay in one place... It's not my nature.""No," She said, downcast, "I guess it's not... You are very... Stand alone.""Stand what?" It was my turn to not understand."Stand alone... It means you will survive with, or without, people. No matter what, you will go on living."She had no idea how close she was to the truth. How could

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she? Even I, who know that no matter what happens, all I can do is take one more step, don't know why.~Fin~

Episode Five: Pecking OrderNothing had gone right to begin with. It seemed like the day had been one accident after another.It started with a mud-like lump of ash, still cool from the night air, falling off the branch that held it. Right onto my head. The one thing I missed about solitude, I decided, was that no one was there to laugh at you when such things happened.That said, I wasn't in solitude anymore. Someone was there to laugh. Lucky me..."Come on Ross, don't be such a grump." Erica said through her failed attempt to suppress her laugh. When I glared at her, she only shook harder. Eventually she had to put her hand on a tree trunk to hold herself up.I bent over and scooped up a handful of the still moist ash fall. I compressed it in my hand with a slight smile. "Think before you laugh at someone," I growled."Ross, what are you-" She became quite serious when she saw me, "No! Don't you dare!"I didn't throw it at her. When she saw this, she sighed in relief. That was, until an entire branch's worth of ash fell on her. The look of shock on her face caught me off guard and I laughed... Then, to my surprise, she started laughing as well."Ok, we're even now?" She took a step towards me. I heard the snap of rope and saw a motion in the trees behind her. Without thinking, I charged at her, dropping my pack on the ground. I collided with her in a full tackle, dragging her to theground as a large log swung through the air behind me. "Ross, what was that for!" She slapped me. I could understand her rage, I had suddenly tackled her, and was now lying on top of her, but understanding didn't help my own anger. I pushed myself to a standing position. "Don'tflatter yourself," I snarled, "There have been plenty of peopleI've wanted to have such encounters with. You are not one ofthem."

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I slowed the log with my hand, "Do you ever think?" I asked, "I just saved your life, passion or desire had nothing to do with it." I froze as a stick snapped somewhere in the underbrush. I drew my sword, "Erica, stay close." I whispered, "And whatever you do, don't put yourself in danger!""Aww... The trap didn't work..." A voice said. Five men came out of the woods in a circle around us. Ash dusted their clothes and seemed to be an inseparable part of their greasy, unkempt hair. I gave each a quick glance as I maneuvered so my back was against the now still log. The day had just gotten a lot worse."You there, ugly with the sword," A man, the leader, I assumed, said with a gap-toothed grin. He alone carried a sword, the others all carried knives. "Hand over the girl and we'll make your death quick. That way, your last thought as you go to hell won't be the vision of someone else enjoying her the way you should have."So much for the 'your money or your life' concept. I raised my sword, "So you were the ones following me in this wood. The infamous Black Skulls, I presume?" I did not wait for an answer, "You can try me, but it will only make your death quicker.""Kill him!" The leader snarled.The first man had a look of pure joy as he rushed me, knife held out. While most villagers and traveling traders would have ran, I made use of his mistake. His charge left his defense wide open. My blade made his chest wide open as it slashed across it. Out of the corner of my eye I saw a flash and I half turned, half lifted my sword in time to block the downward cut of thesecond bandit. I kicked him away and met the third with a sidestep-counterattack combo. He fell to the ground in a crumpled heap, a crimson pool forming around him. Erica took the chance presented by the opening I had made in the circle. She jumped over the body of the bandit I had just killed with grace and took off running. The fourth bandit,who had been on the other side of the log, followed her."No you don't..." The bandit I'd kicked grabbed my boot as I

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made to give chase. I met his eyes with a cold glare and stabbed my sword down. I shook his dying hand off my ankle.I pulled my skinning knife from my belt and balanced in my fingers by the end of the grip. I pulled my arm back and flicked my wrist. The blade spun through the air and lodged itself in the fourth bandit's back."Drop your blade," I turned and faced the leader, "The ground has enough blood on it today without adding yours." The offer was empty, though. The man had just lost and was now in a corner... The caged animal is oftentimes the most dangerous."Go to hell!" The man charged. I deflected his first blow, but he slid his sword to block my counterattack. I grimaced; his fighting style was reminiscent of the Knights that had lived before.Steel clashed on steel, echoing through the still forest. We moved in a slow circle as we parried, deflected and attacked,yet neither of us got ahead. After a relatively short time, we'd worn a circle into the ash with our footsteps, revealing the green grass underneath. Like most knights, his attacks had flair, the result of years of tournaments, more than likely.That was not to say they were for show alone. One thing I had learned over the years was that assuming anything in a fight was a deadly mistake.My luck didn't hold out, though. Perhaps the stars were against me, I couldn't say, it had been years since anyone had seen them to tell. As I deflected a downward slash, the ground underneath me gave way and I fell to one knee in order to keep my balance.I did not raise my sword to block his next attack, rather, I simply raised my left arm to catch the blow. He smiled at meas he started to swing."Ross!" Erica screamed. She rammed the bandit with her shoulder, knocking him down. A brave thing, but now he turned on her."Wench!" He roared, swinging as he leapt forward. I barely had time to pull her away from the attack as I myself rose. Unfortunately, this put me in the line of attack. I grimaced as

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the blade cut into my right forearm. "I'll kill you!""No.. You won't." I said calmly. I swung my sword and he staggered back. I didn't finish there, though he wouldn't have lasted long. I took another step forward. Another slash, another crimson line sprayed upon the ash. And another. And another."Stop it!" Erica finally cried, grabbing me around the waist, "Please! He's dead, they're all dead, isn't that enough? Must it be more terrible?" Tears flowed freely down her cheeks."Do not cry for them," I wiped my blade clean on the cloak ofone of the cleaner bandits, "They made their choice. I made mine, to survive. Remember this lesson, remember it well. Not everything can be solved peacefully. Sometimes people have to die." I removed a necklace from the leader's body asproof of his death, IÆd heard talk of a bounty for these bandits. I faced her and removed my cloak, showing her the steel breastplate and armguards I wore. ôListen to me next time.ö I displayed the gash on my arm for her to see. ôI would have been fine had you not interfered….. Try to take a lesson from this, before you get us both killed. Now, if youÆllexcuse me, I need to try to stop the bleeding.ö"I left her crying in the crimson ash with those words. Maybe they had been a bit cruel, but she had to learn... And no one would cry for her passing, just as they would not mine. The world has no room for idle beliefs or fancies... To live, something must die, that is the Universal Law. That is why there are pecking orders. Those on top must understand this if they are to stay there long.After a while, she got up, and returned to the camp. Neither of us said anything, but she did manage to stitch the wound closed. Sometimes….. I wonder... Wonder about her, her personality. In the broken remnants I face every day, in the years of walking through ash, she alone remains true to whatthe world was before. And I canÆt but ask... Am I here for her? Or….. Is she here for me?~Fin~

Episode Six: Chestnut

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Life had settled itself into a routine after a while. I found myself admitting that Erica was nice to have around, a thought I immediately pushed aside.The last thing I wanted, or needed, was to become 'cozy'.Just when I thought I'd finally gotten used to the constant companionship of another person I was struck with another 'surprise'...It was a bright day, which made the thing stand out even more.There, in the whitish-green brush, without a care in the world, stood a donkey. Even from a distance the thing lookedmiserable and half starved."I wonder if it's tame?" Erica asked me. "I'm guessing, it doesn't look like it's done well out here in the wild," I said. Besides, I wanted to say, Who's ever heard of a wild donkey in the middle of the woods? I started uncoiling a rope."What are you going to do?" "Make a rope bridge," I said, "What do you think? I'm going to hunt a donkey.""No!" She cried. She looked at me with pleading eyes.The donkey let out a startled cry and disappeared into the brush. I cursed under my breath and unslung my bag. "Set up camp." I ordered, putting force into my voice so that she wouldn't question the direction.I'd been looking for a pack animal for a while now. Here, one had been practically free, and that girl seemed to have had some issue with my making use of it. The thought only mademe more bitter at the situation.She certainly complains enough about having to help carry, I thought, not wanting my voice to give me away, though speaking it probably would have made me feel just a little better. What she doesn't realize is I was carrying it all beforeshe came along... And it's not like she minds having clothes, though she does need some clothes that aren't bigger than she is... Or eating the food...I shook my head as I crept through the brush, bitter thoughtswould do me no good right now. I spent most of the day searching the annoyingly endless ash

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covered forest for the donkey. Every rustle I followed turned out to be a rat or other large rodent, but no donkey. Finally, as the sun began to set, I gave up.'Oh, Ross, if I'd known where you were, I would have called you!" Erica said happily as I entered the camp.The donkey let out a nervous bray as we met eyes and took a couple steps back. It quickly looked away from my furious gaze.I was angry. All this time I'd spent and the damn beast had just wandered into the camp. Not only that, but Erica hadn't even thought to make the thing a harness to keep it from wandering away."Ross, no!" She said, alarmed, as I approached the miserablecreature."What is your problem?" I growled, "Why do you insist on hindering me?""Don't kill him!" She pleaded. She even got on her knees in the ash and looked up at me."Get up," I retorted, grabbing her wrist and pulling her to herfeet, "Why would I kill it? It's more useful as a pack beast isn't it, though it doesn't look like it could carry much."The donkey snorted as it dug at the ash with its hoof. I noticed that it kept an eye on me though."I thought..." Erica paused, "You said hunt and...""You really don't ever think, do you?" I took a slow step towards the donkey, which snorted again. "Calm down, you miserable ass." I said. Not the most reassuring choice of words, but I wasn't exactly feeling charitable at the moment.As a reached out, the donkey brayed, giving me a nice view of its crooked teeth. Teeth which promptly reached out and bit my hand. I drew my hand back quickly and glared angrily at the donkey. "Don't make your name out to be dinner, you ungrateful ass. You haven't exactly done well out here, you know."The donkey took a step back. It watched me as it walked, giving me a wide berth, and stood next to Erica, who pet it affectionately on the nose, "His name is Chestnut."I sat down on a relatively thin patch of ash, "'Nuts' is more like it." I replied darkly. "He sure is an ugly ass."

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"I think he's cute." She said defensively. "You don't like him because he doesn't trust you.""No," I started rolling the rope back up, "I don't like him because he has an attitude. Besides," I said with a smile, "You think that's cute, well, then first town we visit I'll find you a mangy, half-starved, rabies ridden dog to keep as well.""That's terrible!" Erica cried, hugging Chestnut, "Maybe that's why he doesn't like you, you're too mean for him! It's not like you're friendly.""I'm actually quite nice," I said, trying to make a harness out of leather strips, "I didn't abandon you, I killed the bandits who wanted to rape you and I didn't kill that ass when it pissed me off. There are things out there that aren't half as nice as I am."She rolled her eyes as she took the harness from me. Chestnut resisted slightly, but let her put it on him. She smiled broadly as she checked the knot on the rope, then presented it to me. "Anything to say now?"I leaned back against a tree, "Yeah, actually, he's your problem. You now have the chore of taking care of him. First thing you might want to do, give him a bath. I won't be able to sleep with the camp smelling like a dirty ass."I smiled to myself as she left. That had taken the smile off her face rather quickly.~Fin~